반응 #1488610

반응 방정식

1-(3-chloro-4-fluorophenyl)ethanone

DMSO

NaH

Trimethylsulfonium iodide

→

crude product

2-(3-chloro-4-fluorophenyl)-2-methyloxirane

용매

THF

—

ice water

THF

반응 조건

후처리

1. 1
   온도heated for another 10 min
2. 2
   온도the reaction mixture is cooled to 0° C
3. 3
   workup.ADDITIONis added dropwise
4. 4
   workup.ADDITIONAfter complete addition
5. 5
   추출extracted in diethyl ether
6. 6
   건조dried over sodium sulfate
7. 7
   농축concentrated at 25° C.

실험 절차

DMSO is added to NaH (1-1.8 equiv.) and heated to 65° C. for 1 h. THF is added at the same temperature and heated for another 10 min. After 10 min., the reaction mixture is cooled to 0° C. Trimethylsulfonium iodide (1-1.2 equiv.) is added and the contents were stirred for 10 min. after which the solution of 1-(3-chloro-4-fluorophenyl)ethanone (1 equiv.) in THF is added dropwise. After complete addition, the reaction mixture is stirred at RT for 2 h; the reaction is monitored by LCMS. After completion, the reaction mixture is poured in ice water, extracted in diethyl ether, dried over sodium sulfate and concentrated at 25° C. to get the crude product.

출처