Methylene plates

From the Endo or eoein methylene plates made as prescribed under Bfish at least two typical colonies, transferring each to an agar slant and a lactose broth fermentation tube. 

Fig. 2. Tic densitometer scans showing the resolution of isoproterenol on a hpflc siUca-gel plate obtained using a mobile phase consisting of 6.8 mM (1 R)-(—)-ammonium-10-camphorsu1fonic acid in 75 25 (v/v) methylene chioride methano1. (a) 254 nm, (b) 275 m, (c) 300 nm.

Aqueous solutions of dyes ean also be employed instead of water. In the ease of hydrophilic dyes such as methylene blue or patent fast blue the transparent background of the TLC/HPTLC plate is stained blue. Pale spots occur where there are nonwetted zones. Dauble [89] detected anion-active detergents in this way on silica gel layers as pale zones on a blue background with palatine fast blue GGN... 

Bicuculline, C2oHi,06N. (Items 1, 9, 10, 13, 14, 18, 20, 23-26, 34, 35, 38 list, p. 169). This alkaloid exists in two forms, m.p. 177° and m.p. 196°, and has [a], ° + 130- 5° (CHCI3). The hydrochloride has m.p. 259° (dec.) and from the methiodide, W-methylbicuculline, plates, m.p. 246°, has been prepared. Bicuculline contains no methoxyl groups it behaves as a lactone and is convertible by alkalis into bicucine, which is possibly the corresponding hydroxy-aeid (see below). It simulates hydrastine in its reactions and differs from that base by CH, indicating that a methylene-dioxy group replaces two methoxyl groups, and this view is supported by comparison of the products of oxidative hydrolysis of the two alkaloids. Both yield hydrastinine (p. 163) as the basic product, but while hydrastine provides as the second product, opianic acid,... 

In like manner lodal (VI), on condensation with 6-nitro-3 4-methylene-dioxyphthalide (IV) yields nitro-a -adlumine (I R = NOj . O. CHa. O. at C and C replaced by 20Me), which crystallises from chloroform-methyl alcohol in orange, rectangular plates, m.p. 180-1° dec.), and on reduction yields the corresponding amino-derivative, bundles of minute needles, m.p. 218-9°. 

Ninety-eight grams of 6-chloro-2-chloromethyl-4-phenylquinazoline 3-oxide hydrochloride were introduced into 600 cc of ice cold 25% methanolic methylamine. The mixture was initially cooled to about 30°C and then stirred at room temperature. After 15 hours the reaction product which precipitated was filtered off. The mother liquor was concentrated in vacuo to dryness. The residue was dissolved in methylene chloride, washed with water and dried with sodium sulfate. The methylene chloride solution was concentrated in vacuo and the crystalline residue was boiled with a small amount of acetone to dissolve the more soluble impurities. The mixture was then cooled at 5°C for 10 hours and filtered. The crystalline product, 7-chloro-2-methylamino-5-phenyl-3H-1,4-benzodiazepine 4-oxide, was recrystallized from ethanol forming light yellow plates, MP 236° to 236.5°C. 

A mixture of 3 grams (0.01 mol) of 7-chloro-1-methyl-5-phenyl-3H-1,4-benzodiazepin-2(1 H)-one 4-oxide, 30 ml of chloroform and 1 ml of phosphorus trichloride was refluxed for one hour. The reaction mixture was then poured on ice and stirred with an excess of 40% sodium hydroxide solution. The chloroform was then separated, dried with sodium sulfate, filtered and concentrated in vacuo. The residue was dissolved in methylene chloride and crystallized by the addition of petroleum ether. The product, 7-chloro-Tmethyl-5-phenyl-3H-1,4-benzodiazepin-2(1 H)-one, was recrystallized from a mixture of acetone and petroleum ether forming colorless plates melting at 125°-126°C. 

After 30 minutes the solid sulfinic acid is separated on a fritted-glass filter. The sulfinic acid is dissolved from the filter by a mixture of 750 ml. of ether and 750 ml, of methylene chloride. The solution is dried over calcium chloride and evaporated to dryness under reduced pressure (bath temperature 25°) (Note 5). The residue is suspended in 50 ml. of water, and small portions of dilute ammonia are added to the well-stirred suspension until it has a pH of 9 (Note 6). Insoluble impurities are separated by filtration, and 2-nitrobenzenesulfinic acid is precipitated from the filtrate by adding 5-ml. portions of 6N hydrochloric acid with cooling the sulfinic acid precipitated by each portion of acid is separately collected on a Buchner funnel (Note 7). The acid, a pale yellow solid, is dried on a clay plate in a vacuum desiccator over potassium hydroxide pellets, m.p. 120-125° (dec.), weight 9.4-14.9 g. (50-80%). If the 2-nitrobenzenesulfinic acid is to be used for the hydrogenation of the next step high purity is required, and it is generally advisable to reprecipitate the acid once more in the same way (Note 8). 

Two-dimensional thin-layer chromatography. This method is used to verify the presence of terminal 5-sultones, terminal unsaturated y-sultone, and terminal 2-chloro-y-sultone, if they are detected in the gas chromatographic determination. After extraction of the neutral oil from the AOS sample, the neutral oil is made up volumetrically to at least a 10% solution in hexane. Of this solution 3 pi is spotted onto a silica gel TLC plate together with standard sultones. It is twice developed with 2-propyl ether and then after turning the plate 90° twice developed with 60/40 n-butyl chloride/methylene chloride. The... 

Films of purified PVCa were cast from methylene chloride solution on quartz plates. The solvent was allowed to slowly evaporate to give smooth, clear films with a thickness of ca. 5.0 nm. Contact angle measurements using water droplets were measured with a standard contact angle goniometer. Samples were photo-lysed in air with polychromatic light from a 150 watt xenon arc. Contact angles were measured after various times of irradiation to monitor the formation of oxidation products at the surface of the polymer films. 

Apply separately to the plate 2.0 pL of each solution, and develop over a path of 15 cm using a mixture of equal volumes of ether and methylene chloride. Allow the plate to dry in air and spray with bromocresol green solution. The principal spot in... 

The various fractions are combined, washed with 20 ml. of cold ether, and dried. Recrystallization from methylene chloride-ether (Note 7) gives 6.0-6.6 g. (62-69%) of 2-hydroxy-3-methyl-isocarbostyril as light orange plates, m.p. 175-180°. Sublimation of this material at 100-110° (0.5 mm.) gives a white product, m.p. 182-184°, with softening at 174° (Note 7). 

Recent chromatographic data indicate that the interactions between the hydrophobic surface of a molded poly(styrene-co-divinylbenzene) monolith and solutes such as alkylbenzenes do not differ from those observed with beads under similar chromatographic conditions [67]. The average retention increase, which reflects the contribution of one methylene group to the overall retention of a particular solute, has a value of 1.42. This value is close to that published in the literature for typical polystyrene-based beads [115]. However, the efficiency of the monolithic polymer column is only about 13,000 plates/m for the isocratic separation of three alkylbenzenes. This value is much lower than the efficiencies of typical columns packed with small beads. 

Chloride salt (la). The pyridinium mesylate from above was dissolved in 200 ml of methylene chloride, and was shaken with 50 ml of saturated NaCl solution in a separatory funnel for ca 2 min. The methylene chloride phase was removed, the brine phase was washed once with 20 ml of methylene chloride, and the organic phases were combined. This procedure was repeated twice using fresh brine. The methylene chloride phase was filtered and evaporated to dryness, affording the crude chloride salt. Recry-stalllzation of the salt from THE/chloroform (ca. 20 1) gives white plates with mp = 192-193 ... 

Fractionation of Porphyrin Methyl Ester. The product mixture (50 mg) was dissolved in methylene chloride (2.0 ml) and treated with excess ethereal diazomethane freshly prepared from p toluenesulfonylmethylnitrosamide (Diazald). The mixture was stirred in subdued light at room temperature. The solvents were evaporated gradually in a fume cupboard. The residue was dried in vacuo and separated on preparative TLC plates to give the methoxyethyl diporphyrin methyl ester whose NMR is shown in Fig. 7 and 8. 

Materials Description. Three CIBA-GEIGY epoxy/hardener systems were studied Araldite 6010/906, Araldite 6010/HY 917 and Araldite 6010/972 with stoichiometries 100/80, 100/80 and 100/27, respectively. Araldite 6010 was a DGEBA epoxy resin. The hardeners 906, HY 917 and 972 were, respectively, methyl nadic anhydride (MNA), methyltetrahydro phthalic anhydride (MTPHA) and methylene dianiline (MDA). These systems were investigated previously for the matrix controlled fracture in composites (6-8). The curing cycles used can be found in (6). The ideal chemical structures of the systems are shown in Table I. Neat resins were thoroughly degassed and cast into 1.27 cm thick plates for preparation of test specimens. 

I. 4-methoxyacetophenone (30 //moles) was added as an internal standard. The reaction was stopped after 2 hours by partitioning the mixture between methylene chloride and saturated sodium bicarbonate solution. The aqueous layer was twice extracted with methylene chloride and the extracts combined. The products were analyzed by GC after acetylation with excess 1 1 acetic anhydride/pyridine for 24 hours at room temperature. The oxidations of anisyl alcohol, in the presence of veratryl alcohol or 1,4-dimethoxybenzene, were performed as indicated in Table III and IV in 6 ml of phosphate buffer (pH 3.0). Other conditions were the same as for the oxidation of veratryl alcohol described above. TDCSPPFeCl remaining after the reaction was estimated from its Soret band absorption before and after the reaction. For the decolorization of Poly B-411 (IV) by TDCSPPFeCl and mCPBA, 25 //moles of mCPBA were added to 25 ml 0.05% Poly B-411 containing 0.01 //moles TDCSPPFeCl, 25 //moles of manganese sulfate and 1.5 mmoles of lactic acid buffered at pH 4.5. The decolorization of Poly B-411 was followed by the decrease in absorption at 596 nm. For the electrochemical decolorization of Poly B-411 in the presence of veratryl alcohol, a two-compartment cell was used. A glassy carbon plate was used as the anode, a platinum plate as the auxiliary electrode, and a silver wire as the reference electrode. The potential was controlled at 0.900 V. Poly B-411 (50 ml, 0.005%) in pH 3 buffer was added to the anode compartment and pH 3 buffer was added to the cathode compartment to the same level. The decolorization of Poly B-411 was followed by the change in absorbance at 596 nm and the simultaneous oxidation of veratryl alcohol was followed at 310 nm. The same electrochemical apparatus was used for the decolorization of Poly B-411 adsorbed onto filter paper. Tetrabutylammonium perchlorate (TBAP) was used as supporting electrolyte when methylene chloride was the solvent. 

The steroids below are spotted onto a silica gel TLC plate. The plate Is developed in methylene chloride/ether/methanol/water (77 15 8 1.2) and under UV light has the appearance shown in Figure 13.4. From your knowledge of the polarity of organic molecules, match the steroids to the spots on the TLC plate shown in Figure 13.4. 

Antibacterial activity. Methylene chloride extract of the dried aerial parts of the plants, on agar plate at a concentration of 1 g/mL, was active on Bacillus subtilis L Methanol extract of the shade-dried plant, on agar plate at a concentration of 0.6 mg/mL, was inactive on Staphylococcus aureus. A concentration of 10 mg/mL was inactive on Escherichia coli and Pseudomonas aureugi-nosab L... 

Dorzolamide ean be chromatographed using silica gel TLC plates, and a mobile phase of 80 20 1 methylene chloride methanol ammonia. Visualization can be effected by either viewing the developed plate under ultraviolet light, or by exposing the developed plate to iodine vapor. The R, of dorzolamide is approximately 0.62. 

In every analysis of propellants an extraction must be performed. The latest description of the method used by the US Armed Forces is of 1971 (Ref 5). Roweg, Soxhler or equivalent extractor must be used and as extracting solvent, diethyl ether or anhydrous methylene chloride. Proceed as follows Transfer an accurately weighed sample of propint, about 5g, to the thimble of the extractor and add prescribed solvent to the tared extraction flask. Insert the open lower part of the extractor into die neck of the extraction flask and insert thru the upper opening of the extractor die bottom opening of the reflux condenser. Assemble the apparatus on the hot plate, and adjust the temperature so that the solvent drips from die condenser at the rate of 2—3 dtops per second. Extract for a time which experience or preliminary work has shown to be adequate for the type of sample. It takes 3 to 20 hours and for Roweg extractor 2—3 times faster chan for Soxhlet. 

Mixtures of PEI/epoxy monomer and PEI/BPACY monomer were prepared by dissolving PEI and thermoset monomers in methylene chloride at room temperature and evaporating the solvent. The epoxy monomer/PEI solution was heated on a hot plate to 140°C, and stoichiometric amounts of DDS were added while stirring for about 7 min. For the catalyzed system, 2-methyl imidazol catalyst was also added. 

Many tests are described in Ref 14 and following is the abstract of some tests Qualitative Tests. Pulverize the proplnt to test, extract it. with ether on methylene chloride (as described in MIL-STD-286A, Method 104.1 or in Vol 2 of Encycl, p C131-L) and evaporate the solvent using a stream of dry air. Place ca 1 mg of this residue on a spot plate and add a few drops of the reagent, such as de-... 

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