On silica gel

Hydrocarbon groups (FIA method) NF M 07-024 ISO/DIS 3837 ASTM D 1319 Chromatography on silica gel with fluorescent indicators... 

Fig. XVI-6. Nuclear correlation times for water adsorbed on silica gel. (From Ref. 94.)...

The irradiation of tetra-/-butylcyclopentadienone with 254 nm light at 77 K produced a tricyclopentanone which, upon extended irradiation, lost carbon monoxide. Tetra-f-butyltetrahedrane was formed. This derivative of the second fundamental hydrocarbon of molecular formula (CH), namely tetrahedrane, is stable at room temperature and could be isolated after chromatography on silica gel in crystalline form (G. Maier, 1978). 

A solution of benzyl indole-5-carboxylate(1.0g, 3.98 mmol) and methyl 4-(bro-momethyl)-3-methoxybenzoate (2.06 g, 7.97 mmol) in dry DMF (10 ml) was heated at 80°C for 24 h. The reaction solution was cooled, poured into water (100 ml) and the product extracted with EtOAc (3 x 75 ml). The extract was washed with water and brine and dried over MgSO, . The product was obtained by evaporation of the solvent and purified by chromatography on silica gel using 1 4 EtOAc/hexane for elution. The yield was 1.11 g (32%) and some of the indole (30%) was recovered unreacted. 

Potassium hydride (1 eq.) was washed with hexanes and suspended in anhydrous ether at 0°C. 7-Bromoindole was added as a solution in ether. After 15 min, the solution was cooled to — 78°C and t-butyllithium (2 eq.) which had been precooled to — 78°C was added by cannula. A white precipitate formed. After 10 min DMF (2 eq.) was added as a solution in ether. The reaction mixture was allowed to warm slowly to room temperature and when reaction was complete (TLC) the suspension was poured into cold 1 M H3PO4. The product was extracted with EtOAc and the extract washed with sat. NaHCOj and dried (MgS04). The product was obtained by evaporation of the solvent and purified by chromatography on silica gel (61% yield). 

To a stirred ice-cold solution of ethyl 3,6-dihydro-5-hydroxy-8-methyl-6-(phenylsulfonyl)benzo[l,2-b 4,3-b ]dipyrrole-l-carboxylate (368 mg, 0.85 mmol) in TEA (3ml) was added EtjSiH (1.5 ml), After 15 min the solution was allowed to come to room temperature and stirred for an additional 2h. The solution was evaporated in vacuo and the residue dissolved in CH2CI2 (10 ml), washed.with aq. NaHCOj and dried over MgS04. The solution was mixed with AcjO (1ml) and CH2C12 (1ml) and kept at room temperature for 2 h. The reaction mixture was evaporated and the residue purified by chromatography on silica gel using CHjClj-EtOAc (3 1) for elution. The product (271 mg) was obtained in 71 % yield. 

To a solution of indoline (20 mM in MeOH) was added Co(salen) (0.10 equiv.) and O2 was bubbled through the suspension at 25°C. After 1 h the suspension became homogeneous and the solvent was removed in vacuo and the product purified by chromatography on silica gel. 

FIG. 25-7 Eq nilibriiim partial pressures for certain organics on silica gel. 

Brombenztiazo (BBT) is known to be one of the best reagents for extraction-photometric determination of cadmium(II). The reagent also fonus complexes with Co(II), Cu(II), Fe(II), Ni(II), Zn(II). The aim of this work was to develop a solid-phase reagent on the base of BBT immobilized on silica gel for sorption-spectroscopic and visual test determination of Cadmium, and also for soi ption-atomic-adsoi ption determination of total heavy metals contents in natural waters. 

A simple, rapid, precise and economical High Performance Thin Layer Chromatographic (HPTLC) method has been developed and validated for determination of Alprazolam and Melatonine in its pharmaceutical preparation. It was performed on silica gel 60 Thin Layer... 

It is known that Selenium catalyzes reaction of some dye reduction by Sulphide. On this basis spectrophotometric and test-techniques for Selenium determination are developed. Inefficient reproducibility and low sensitivity are their deficiencies. In the present work, solid-phase reagent on silica gel modified first with quaternary ammonium salt and then by Indigocarmine was proposed for Selenium(IV) test-determination. Optimal conditions for the Selenium determination by method of fixed concentration were found. The detection limit of Se(IV) is 10 ftg/L = 2 ng/sample). Calibration curve is linear in the range 50-400 ftg/L of Se(IV). The proposed method is successfully applied to the Selenium determination in multivitamins and bioadditions. 

Dihydro-2(3H)-turanthlone (3).2 Butyrolaclone 1 (0 86 g. 10 mmoO and [2,4-bis(4-methoxyphenyl)-l, 3-dilhia 2,4-diphospheiane-2,4-disui(ide) 2 (2 02 g, 5 mmol) in PhMe (10 mL) were heated to reflux until no more starling malenal was detected (TLC or GC) After cooling, the solvent was stripped off and the mixture was punlied on silica gel using CH2CI2 as eluent to afford 3, mp 96-97 C... 

General procedure. LaNIs ingot (3 g) in an autoclave was evacuated at 0.1 mm, heated to 200°C under Hz at 30 atm for 10 min. After cooling to 20°C, Itie operation was repeated five times. The autoclave was cooled in dry ice-acetone, Hg was released and Ng was Introduced. The organic compound (1 mmol) m THFJ4eOH (2 1) (5 mL) was added at -78°C with stirring. Tt mixture was stirred under Ng at 0°C and then at 20°C. The catalyst was filtered, the filtrate concentrated and the residue purified by preparative TLC on silica gel. 

This ester is formed by standard procedures and is readily cleaved with Pd(Ph3P)4 in CH2CI2 to form trimethylsilyl esters that readily hydrolyze on treatment with water or alcohol or on chromatography on silica gel (73-98% yield). Amines can be protected using.the related carbamate. ... 

A-(9-Acridinyl)maleiinide (NAM) [49759-20-8] M 274.3, m 248 , 255-258 . Purified by chromatography on silica gel using CH2CI2 as eluant. Evaporation of pooled fractions that gave the correct NMR spectra gave a solid which was recrystd from Me2CO as pale yellow prisms. IR v (nujol) 1710 (imide) UV (MeOH) (nm), (e M- cm ) 251 (159 500), 343 shoulder (7 700), 360 (12 400) and 382shoulder (47... 

Anthrarufin [l,5-dihydroxy-9,10-anthraquinone] [117-12-4] M 240.1, m 280 (dec), pKj 9.90, pK 11.05. Purified by column chromatography on silica gel with CHCl3/Et20 as eluent, followed by recrystn from acetone. Alternatively recrystd from glacial acetic acid [Flom and Barbara J Phys Chem 89 4489 1985]. 

Bismethylaminoanthraquinone (Disperse Blue 14) [2475-44-7] M 266.3, A,max 640 (594)nm. Purified by thin-layer chromatography on silica gel plates, using toluene/acetone (3.1) as eluent. The main band was scraped off and extracted with MeOH. The solvent was evapd and the dye was dried in a drying pistol [Land, McAlpine, Sinclair and Truscott J Chem Soc, Faraday Trans I 72 2091 7976]. 

Purified by chromatography on silica gel in CHCl3/pet ether (1 2) followed by crystn from aqueous EtOH. [Phillips and Cohen J Am Chem Soc 108 2023 7956.]... 

Purified by TLC on silica gel with EtOAc-pet ether (b 60-80°) (15 85), and recrystallised from MeOH or CgH6. [NMR Wamhoff Can J Chem 42 1664 1964, Ramage and Whitehead J Chem Soc 4336 1954.]... 

Carbon soot from resistive heating of a carbon rod in a partial helium atmosphere (0.3bar) under specified conditions is extracted with boiling C H or toluene, filtered and the red-brown soln evapd to give crystalline material in 14% yield which is mainly a mixture of fullerenes C q and C70. Chromatographic filtration of the crude mixture with allows no separation of components, but some separation was observed on silica gel... 

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