반응 #1470435

반응 방정식

di-n-butyl chlorophosphate

dichloromethane

Isobutanol

→

di-n-butyl isobutyl phosphate

용매

pyridine

반응 조건

후처리

1. 1
   여과The pyridinium hydrochloride was filtered off
2. 2
   세척the solution was washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (25×250 mL)
3. 3
   건조The organic phase was dried over anhydrous magnesium sulfate for 12 hours
4. 4
   여과Filtration of the drying agent
5. 5
   기타followed by the removal of the solvent

실험 절차

A solution of di-n-butyl chlorophosphate (130.3 g, 0.57 mole) in 600 mL of dichloromethane containing 55.37 g (0.70 mole) of pyridine was cooled to 0° C. Isobutanol (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 was washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (25×250 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 di-n-butyl isobutyl phosphate as a clear colorless liquid. Distillation of the crude product (68° C. at 0.02 torr) gave 125 g of 94.8% di-n-butyl isobutyl phosphate (DBIBP).

출처