반응 #1470436

반응 방정식

diisobutyl chlorophosphate

pyridine

n-Butanol

→

n-butyl diisobutyl phosphate

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise over 1 hour
2. 2
   여과The pyridinium hydrochloride was filtered off
3. 3
   세척the solution washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (2×250 mL)
4. 4
   건조The organic phase was dried over anhydrous magnesium sulfate for 12 hours
5. 5
   여과Filtration of the drying agent
6. 6
   기타followed by the removal of the solvent

실험 절차

A solution of diisobutyl chlorophosphate (130.3 g, 0.57 mole) in 600 mL of dichloromethane and 55.37 g (0.70 mole) of pyridine was cooled to 0° C. n-Butanol (42.25 g, 0.57 mole) was added dropwise over 1 hour. The formation of a white precipitate was immediately observed. The reaction mixture was then stirred for 24 hours at room temperature. The pyridinium hydrochloride was filtered off and the solution washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (2×250 mL). The organic phase was dried over anhydrous magnesium sulfate for 12 hours. Filtration of the drying agent, followed by the removal of the solvent using a Roto-vap, yielded n-butyl diisobutyl phosphate as a clear colorless liquid. Distillation of the crude product (68° C. at 0.02 torr) gave 125 g of 96% n-butyl diisobutyl phosphate (BDIBP).

출처