Butanol shake extraction

The extracted aqueous solution is covered with butanol and the pH adjusted to 2 by the addition of N HCI. The acidified aqueous phase is extracted with butanol, the pH of the aqueous phase being adjusted to pH 2 each time. The combined butanol solutions which contain the free acid, a-carbobenzyloxyaminobenzylpenicillin, are washed with water, and are then shaken with water to which sufficient 3% sodium bicarbonate has been added to bring the aqueous phase to pH 7. The process of washing and shaking i repeated with fresh water and bicarbonate solution. The combined aqueous solutions are washed with ether and then are evaporated under reduced pressure and low temperature. The product, the sodium salt of a-carbobenzyloxyaminobenzylpenicillin, is obtained as a yellow solid in a yield of 65%. 

A simplified procedure for detecting the M. aeruginosa toxins was devised. A 20.0 mg sample of lyophilized cells was extracted for 1 hr with 1 ml of 38% ethanol, 5% n-butanol, 50 mM ammonium acetate pH 6.0, shaking the suspension manually for a few seconds several times. The suspension was then centrifuged (5 min at 12,000 Xg). 

Bulk Nandrolone (19-Nortestosterone) TLC Dissolve in water, pH 5.5-9.0, extract with CHCI, Silica (activated) MeOH-ammoniated butanol, butanol prepared by shaking 100 ml butanol with 60 ml NH4OH, discard 1% lower layer Ferric chloride USP 23 [2,3,10,958, 1133,1134] [5]... 

All sediment samples were pre-extracted first with 40 mL of methanol or butanol and subsequently with solutions of hexane/acetone (1 1 v/v) by means of shaking for 24 h in the dark and ultrasonication at 2 x 450 W (Badelin, Berlin, FRG) in a water bath for 30 minutes. Each extraction step was followed by centrifugation at 1800 x g and the combined extract was reduced in volume by rotary evaporation. 

Powdered drug (1 g) is extracted with 10 ml 50% methanol by healing under reflux for ElcutherococcI 15 min after cooling, 15 ml water-saturated n-butanol is added. After shaking for 5 min, radix, Visci albi the butanol phase is separated and evaporated to approximately 1 ml 20-40 pi is used hcrba for TLC. 

Powdered drug (1 g) is extracted for 2h with 20 ml water, with occasional shaking. For Enrichment further enrichment of the diterpene glyco.sides, the extract is shaken with 20ml n-butanol and the n-butanol-phase separated. The filtrate is evaporated to 3 ml and 20 [il i.< used for TI.C. 

Typical procedure. Cyano-tert-butyloxycarbonyl-glycine (CyOC-Cly-OH) 568 [404] To a solution of cyano-tert-butanol 566 (10 g, 100 mmol) and pyridine (10 g, 125 mmol) in dichloromethane (150 mL) at —40 °C was added phosgene (40 mL, 600 mmol) (for a safe source, see Chapter 7), precooled to —70 °C. The mixture was stirred overnight at room temperature and then washed with ice-cooled 1 n HQ and twice with ice/water. The organic layer was successively dried by shaking it several times with fresh sodium sulfate (all aqueous phases and the sodium sulfate were extracted twice with dichloromethane). The solvent was evaporated in vacuo at 20 °C (bath temperature) to afford 17 g (quantitative) of crude cyano-ferf-butyl chloro-formate 567. Crude chloroformate 567 was dissolved in THF (100 mL) and the so-... 

Procedure. One drop of the test solution (in 0.1 M nitric acid) is mixed with one drop of a 0.03 % solution of the reagent in a micro test tube. The blue-green complex can be extracted by shaking with a few drops of butanol containing 3 % tribenzylamine. A blue-green color in the organic layer indicates the presence of plutonium. 

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