H Methanol

FIG. 13-63 (Continued) Batch distillation paths, (h) Methanol-acetone-chloroform system. 

Tea. A 4-g sample is homogenized and soaked with 16 mL of distilled water for 2 h. Methanol (100 mL) is added to the mixture and shaken for 30 min. The extract is filtered through a Celite layer (1-2 cm thickness) under vacuum. The filter cake and vessel are washed twice, each with 25 mL of methanol. The combined filtrates are transferred to a separatory funnel. ... 

Phosphorus acid (260 mg, 3.17 mol) was placed into a 250-ml, threenecked, round-bottomed flask suspended in an oil bath. The flask was equipped with a three-way adapter, carrying a pressure-equalizing addition funnel, a reflux condenser with a drying tube, a mechanical stirrer, and a thermometer. Acetonitrile (33 g, 0.80 mol) was introduced to the reaction flask dropwise over a 2-h period while the phosphorous acid was agitated and maintained at a temperature of 138 to 142°C. After completion of the addition, the reaction mixture was maintained at that temperature for an additional 12 h. Methanol was then added to precipitate the pure l-aminoethane-l,l-diphos-phonic acid (13.9 g, 85%), which exhibited spectral and analytical data in accord with the proposed structure. 

General Procedure A (esterification of amine) 1 A 50 wt% methanol solution of methyl acrylate (17 g, 0.2 mol) was added to the methanolic solution of Jeffamine T-3000 (100 g, 0.033 mol). This reaction was allowed to stir at room temperature under a nitrogen atmosphere for 48 h. The reaction was then heated to 50°C for 1 h. methanol and excess methyl aerylate were removed by rotary evaporator. After the dialysis using membrane filter with a MWCO of 3 D in methanol, the product was obtained as a yellow viscous oil (6 g, 98%). H NMR (CDCl, 5),... 

NH3/NH4C1 COOH Oberschufi an NH3/NH4C1. 28% NHs(HaO)/KH a. Autoklav 180 40 h Methanol/H2S04 RUckfluQ 36 h 3-Amino-5-hydroxy-benzoesdure- methylester 75 2... 

Pivalonitrile (33.2 g) and t-butyl chloride (44.4 g) were added under nitrogen over 1 h to a well-stirred suspension of sodium sand (18.4 g) in a mixture of light petroleum (80 ml), THF (20 ml) and methanol (1ml), keeping the reaction temperature between 15 and 20°C during addition. The mixture was stirred for 3h. Chlorobenzene (2 g) in THF (5 ml) was added dropwise over 10 min, and stirring continued (1 h). Methanol (20 ml) was cautiously added over 0.5 h, followed by water, until clear phases separated. The aqueous phase was extracted with ether (3 X 50 ml). The combined organic phases were dried and concentrated under reduced pressure. Distillation afforded the pure imine (63%), b.p. 62-63°C/19 torr. 

A solution of one part of kanamycin B-3 -phosphate, 10 parts by volume of bis(trimethylsilyl)acetamide, 2 parts by volume of trimethylchlorosilane and 0.4 part of triphenylphosphine is heated at 115°C for 30 h. After cooling, the reaction mixture is concentrated under reduced pressure, and to the concentrate is added 100 parts by volume of methanol and 50 parts by volume of water, and then the mixture is stirred for 1 h. Methanol is removed by distillation, and ethyl acetate-soluble portion is removed. The water layer is run onto a column of 60 parts by volume of cation-exchange resin [Amberlite CG-50, NH4+-form], The column is washed with 200 parts by volume of water, and fractionated by linear gradient method with 600 parts by volume of water and 600 parts by volume of 0.5 N-aqueous ammonia, each fraction being 10... 

To a mixture of cholesterol (0.77 g, 2 mmol) in dichloromethane (10 ml) were added pyridine (0.6 ml, 8 mmol) and phenoxythiocarbonyl chloride (0.4 ml, 2.2 mmol). After 2 h, methanol (1 ml) was added, and the mixture was washed with 1 M HC1 aq. solution twice, then dried over Na2S04. After filtration and removal of the solvent, the residue was recrystallized from acetone to give phenyl thiocarbonate in 95% yield. 

Compound 50c was obtained in ca. 25% yield as a precipitate from the acid-catalyzed condensation of pyrogallol and isovaleraldehyde. No evidence of any hexamer was found in the solid material. To convert this material into the hexamer (50c)6, the original precipitate can be dissolved in Et20, acetone, or methanol, with a few drops of nitrobenzene or o-dinitrobenzene, followed by crystallization upon slow evaporation. The hexamer may also be obtained by thermal treatment of the initial precipitate or the initial filtrate. The product in the initial filtrate may be converted into hexamer by extraction in Et20, followed by evaporation to dryness with subsequent dissolution in methanol. The methanol solution is then heated to 120-150 °C for at least 12 h. Methanol may be removed under vacuum to yield a red-brown solid. Colorless hexameric spherical capsules are obtained from this solid utilizing the crystallization procedure described for the initial precipitate. 

Loss on Drying Determine as directed under Loss on Drying, Appendix IIC, drying a sample at 105° for 2 h. Methanol, Ethanol, and Isopropanol... 

A solution of pentachlorophenylmagnesium chloride" is prepared from hexachlorobenzene (66 g, 0.23 mol) and magnesium (8.44 g, 0.35 mol) in a mixture of THF (150 ml) and benzene (150 ml) (HAZARD toluene would be preferable). The solution is heated to reflux, and ethyl formate (40 ml, excess) is added by syringe at such a rate that the exothermic reaction maintains refluxing. The mixture is stirred as it is allowed to cool to room temperature during 1 h. Methanol (20 ml) is added, and the solvents are evaporated. The resulting dark-brown residue is washed with hydrochloric acid, methanol and ethyl acetate, and then recrystallized from 4 1 toluene-pyridine, to give bis(pentachlorophenyl)methanol (35 g, 29%). 

In a report by Nakahara et al., the extraction efficiency of various methods for 6-AM and morphine was compared. Finely cut hair samples were placed into solutions of methanol, 0.1 M HCl, methanol-5 M HCl (20 1), helicase, or methanol-trif-luoroacetic acid (TFA) (9 1). Extraction was performed overnight following ultrason-ication for 1 h, except for the methanol extract, which was sonicated for 14 h. Methanol-TFA was found to be the best solvent for extracting 6-AM and morphine with minimal hydrolysis and maximum extraction efficiency. Nakahara et al. noted that heroin was not detected in heroin users hair by this method, possibly due to hydrolysis to 6-AM. The extraction rates of 6-AM and morphine from heroin users hair with methanol-TFA reached a plateau after 8 to 10 h. 

Year Catalyst Syngas pressure fbar) H2/CO ratio Temp. rc> Time (h> Methanol conv. m Ethanol selectivity (%) Ref. 

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