반응 #61384

반응 방정식

1,3-dichloro-propan-2-ol

diisopropylamide

1-fluoro-2-nitro-benzene

→

title compound

1-(2-Chloro-1-chloromethyl-ethoxy)-2-nitro-benzene

용매

THF

water

반응 조건

후처리

1. 1
   workup.STIRRING8.5 mmoles) and stirred at room temperature overnight
2. 2
   추출extracted with EtOAc
3. 3
   세척washed with brine
4. 4
   건조dried over Na2SO4
5. 5
   농축concentrated under vacuum

실험 절차

A solution of 1,3-dichloro-propan-2-ol (1.29 g, 10 mmoles) in THF, under nitrogen, was cooled to 0° C., treated dropwise with llithium diisopropylamide (LDA) (5 ml, 2M solution in hexanes, 10 mmoles), while maintaining the temperature constant at 0° C., stirred at 0° C. for 15 minutes, treated with 1-fluoro-2-nitro-benzene (1.2 g ml, 8.5 mmoles) and stirred at room temperature overnight. The reaction mixture was diluted with water and extracted with EtOAc. The extracts were combined, washed with brine, dried over Na2SO4, and concentrated under vacuum, to afford the title compound as an off-white solid (2.0 g, 8 mmoles), identified by HNMR analysis.

출처