반응 #56364

반응 방정식

HCl

1-methylethyl 2.2-dichloro-2[(1-methylethoxy)phenylphosphinyl]acetate

n-butyl lithium

→

1-methylethyl 2-chloro-2[(1-methylethoxy)phenylphosphinyl]acetate

수율 78.0%

용매

ether

hexane

반응 조건

후처리

1. 1
   온도to warm to -10°
2. 2
   기타The phases were separated
3. 3
   세척the organic phase washed with water
4. 4
   기타The solution was then dried

실험 절차

To a solution of 7.1 g of 1-methylethyl 2.2-dichloro-2[(1-methylethoxy)phenylphosphinyl]acetate in 150 ml of ether was added 14 ml of a solution of 1.6 M n-butyl lithium in hexane at -70° over 15 minutes. The solution was then allowed to warm to -10° before adding 60 ml of 0.5 M aqueous HCl solution at -10° to 0°. The phases were separated and the organic phase washed with water then 5% NaHCO3 solution. The solution was then dried and stripped to give 5.0 g of 1-methylethyl 2-chloro-2[(1-methylethoxy)phenylphosphinyl]acetate as a light yellow oil ND25 1.5057.

출처