Methanolic ammonia solution

Methanol — ammonia solution (25%) — glacial acetic acid (8 -t-1 + 1). 

In some cases, e.g. the detection of antioxidants [6], the plate is heated to 105 °C for 5 min after being sprayed and the still hot plate placed immediately in an ammonia-vapor chamber. The blue color of the tryptamine derivatives is also stabilized by spraying afterwards with a 5% methanolic ammonia solution [12]. 

Popova and colleagues47 carried out TLC of oxidation products of 4,4 -dinitrodiphenyl sulphide (the sulphoxide and sulphone) on silica gel + a fluorescent indicator, using hexane-acetone-benzene-methanol(60 36 10 l) as solvent mixture. Morris130 performed GLC and TLC of dimethyl sulphoxide. For the latter, he applied a 6% solution of the sample in methanol to silica gel and developed with methanol-ammonia solution(200 3), visualizing with 2% aqueous Co11 thiocyanate-methanol(2 1). HPLC separations of chiral mixtures of sulphoxides have been carried out. Thus Pirkle and coworkers131-132 reported separations of alkyl 2,4-dinitrophenyl sulphoxides and some others on a silica-gel (Porosil)-bonded chiral fluoroalcoholic stationary phase, with the structure ... 

Induced fluorescence (X, > 430 nm, cut off filter) by thermal treatment of the chromatogram, the fluorescence increased by a factor of 2.5 by dipping in a solution of Triton X-100 — chloroform (1+4). Working range 2-50 ng substance per chromatogram zone. Prewashing the layers with methanol-ammonia solution (25%) (50+ 50) increased the precision. 

TLC plates Aluminium oxide 150 F254 (Merck) before application of the samples the layer was developed twice to its upper edge with methanol — ammonia solution (25 %) (50 + 50) to pre-cleanse it and then dried after each development at 120 °C for 30 min. 

Mobile phase Chloroform - methanol - ammonia solution (32%) (204-164-10). 

Note Under the conditions employed emetine and cephaeline were not well separated but there was good resolution of the subsidiary alkaloids of the ipecacuanha tincture (Fig. 1). The separation and quantitative determination of the main alkaloids (Fig. 2) can be carried out under the following conditions Ascending, one-dimensional development in a trough chamber with chamber saturation layer HPTLC plates Silica gel 60 (Merck) mobile phase dichloromethane — methanol — ammonia solution (25%) (34+6+1) migration distance 6 cm running time 13 min h/ f cephaeline 65-70 emetine 75-80. 

Mobile phase Chloroform — methanol — ammonia solution (32%) (20-1-16-1-10). 

Normal phase silica column Chloroform-methanol-ammonia solution (86.8 12.5 0.7) 254 nm Assay of primaquine and hepatic targeting neoglycoalbumin-primaquine in whole blood and liver of mouse by reversed-phase HPLC. [105]... 

An exceptionally short synthesis of grassularine-1 133 was reported recently by Horne and coworkers [95]. This approach utilized intermediate oxotryptamine 146, which had been prepared previously as part of another synthesis [96]. Condensation of 146 with dimethylcyanamide produced 147, which was prone to oxidation, and was only stable as its hydrochloride salt (Fig. 41). This sensitivity to oxidation was utilized in the key reaction step in which oxidative dimerization to give 148 was accomplished by stirring 147 in methanolic ammonia solution at room temperature for 1 day. Continued stirring under these conditions for another 5 days eventually resulted in the production of 149 in 60% yield directly from 147. Hydrolysis of 149, which required forcing conditions (12-h reflux in a mixture of ethanol and 6M HC1), but nevertheless proceeded in 95% yield, completed this synthesis of grassularine-1 133. 

The lactone derivative 158 obtained from D-ribono- 1,4-lactone afforded (—)-(i )-angelica lactone (159a) upon treatment with methanolic ammonia solution (6). In a similar way, Font and coworkers (207) synthesized (+)-(S)-... 

The appropriate aromatic or heteryl- aldehyde (2 mmol freshly distilled if liquid) and 25% methanolic ammonia solution (5 mL) were added to a solution of 1-naphthol (1 mmol) in absolute MeOH (5 mL).The mixture was left to stand at ambient temperature for 2 days, during which oily products separated. The solvent was evaporated and the crade oily products were purified by column chromatography. The physical data for the compounds la-f are listed Table 39.1. 

A previously reviewed method was applied for OTC, TC, CTC, DXC, and DMC analysis in tissue and egg samples however, further optimization and improvement were necessary. The optimal recoveries from tissue were obtained using succinate buffer and MeOH as a depro-teinization agent. The eluate from the MCAC column was acidified and further purified on an Empore disk equipped with a poly(styrene-divinylbenzene)-RP sulphonated membrane previously activated with MeOH and hydrochloric acid (pH 1.0). The elution of TCs was done with methanolic ammonia solution. The extract was evaporated under vacuum and reconstituted in oxalic acid solution. Even though the stability of TCs is poor under alkaline conditions, no influence on the recovery was observed (59-76% with RSD < 6.5% for kidney samples) (26). 

N2,9 -Acetyl-9-(l,3-dihydroxy-2-propoxymethyl)guanine (721.9 mg, 2.4 mmol) was stirred with 50 ml of methanolic ammonia solution (methanol saturated with ammonia at 0°C) for 17 hours at 21°C. The solution was concentrated to a white solid and the residue recrystallized from methanol to give 582.3 mg of 9-(l,3-dihydroxy-2-propoxymethyl)-guanine, melting point 250°C (decomp.). 

Chlorotriazine (150) could be converted to the corresponding 3-aminotriazine (146a) in a yield of 86% by treatment with a saturated methanolic ammonia solution. Subsequent reaction of the... 

The reaction of perfluoroalkylated a, -unsaturated phosphonatcs such as 6 with saturated, methanolic ammonia solution affords diethyl 2-amino-2-(perfluoroalkyl)phosphonates (e. g., 8) and methanolic adducts such as 7. Reaction with benzylamine yields diethyl 2-benzylamino-2-(perfluoroalkyl)phosphonates (e. g., 9) which, upon hydrogenation, also give diethyl 2-amino-2-(perfluoroalkyl)phosphonates. ... 

Pyridazine can be obtained in reasonable yield from the readily available maleic hydrazide (7) which is converted into 3,6-dichloro-pyridazine (8) and upon hydrogenolysis of both chlorine atoms pyridazine is formed. Hydrogenolysis over palladium-charcoal catalyst in the presence or absence of sodium hydroxide at atmospheric pressure gives pyridazine in low yield. If the catalytic hydrogenation is performed under pressure and in the presence of ammonia or in aqueous methanolic ammonia solution at ordinary pressure, pyridazine can be obtained in 60 and 67.5% yield, respectively. 

Post-column techniques tend to be more complex because additional instrumentation e.g. a pump and mixing chamber are required. However, some solutes can be made to fluoresce by simply modifying the eluant pH. This approach has been used for the analysis of quinine and rodenticides. With the former, the compound is chromatographed under basic conditions and then made fluorescent by the addition of perchloric acid after it elutes from the column. With rodenticides, chromatography under acidic conditions is needed and they are then made to fluoresce by changing the pH of the eluate to pH 11 by mixing with a methanol/ammonia solution. 

Solasodine glycosides were applied to TLC plates and developed with chloroform-methanol-ammonia solution (7 2.5 1). A developed TLC plate was dried and then sprayed with blotting solution mixture of isopropanol-methanol-water (5 20 40, by volume). It was placed on a stainless-steel plate, then covered with a PVDF membrane sheet. After covering with a glass microfiber filter sheet, the whole plate was pressed evenly for 45 s with a 130°C iron, as previously described [11], but with a modification. The PVDF membrane was separated from the plate and dried. 

The first total synthesis of amiclenomycin, an inhibitor of biotin biosynthesis, was completed by A. Marquet and co-workers. In order to prove its structure unambiguously, both the cis and trans isomers were prepared. The L-amino acid functionality was installed by a Strecker reaction using TMSCN in the presence of catalytic amounts of Znla. The resulting O-TMS protected cyanohydrin was exposed to saturated methanolic ammonia solution, which gave rise to the corresponding a-amino nitrile. Enzymatic hydrolysis with immobilized pronase afforded the desired L-amino acid. 

Solvent system Toluene + methanol (90 + 14) Ethyl acetate + methanol + ammonia solution (85 + 10 + 5) Ethyl acetate + methanol + ammonia solution (85 + 10 + 5) Methanol + water (72 + 28)... 

---