반응 #1572575

반응 방정식

4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one

P2S5

water

ethyl acetate

→

4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione

수율 60.1%

용매

pyridine

반응 조건

후처리

1. 1
   건조the separated organic layer was dried over Na2SO4
2. 2
   농축concentrated in vacuum
3. 3
   기타the residue was purified by CombiFlash (DCM:MeOH=20:1)

실험 절차

A solution of 4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (3.2 g, 19.6 mmol) and P2S5 (5.2 g, 23.5 mmol) in pyridine (100 mL) was heated at 120° C. and stirred for 30 min. After being cooled to room temperature, water (100 mL) and ethyl acetate (200 mL) were added, the separated organic layer was dried over Na2SO4, concentrated in vacuum, and the residue was purified by CombiFlash (DCM:MeOH=20:1) to give 4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione as a yellow solid (2.1 g, 59%). LRMS (M+H)+: 177 m/z.

출처