Sodium borohydride → 5,6-dihydro-4-oxo-4H-pyrrolo[1,2-a]-thieno[2,3-f][1,4]diazepine

HRID 654064노트

반응식

HRID 654064 반응식
[BH4-].[Na+].N1([CH:9]2[NH:15][C:14](=[O:16])[C:13]3[S:17][CH:18]=[CH:19][C:12]=3[N:11]3[CH:20]=[CH:21][CH:22]=[C:10]23)CCCCC1>CO>[O:16]=[C:14]1[C:13]2[S:17][CH:18]=[CH:19][C:12]=2[N:11]2[CH:20]=[CH:21][CH:22]=[C:10]2[CH2:9][NH:15]1

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 10850843HCID 10850843, 화합물

생성물 1

HCID 106320145,6-dihydro-4-oxo-4H-pyrrolo[1,2-a]-thieno[2,3-f][1,4]diazepine수율 84%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1 g (0.0028 mol) of sodium borohydride is added in small portions to a solution of 2 g (0.007 mol) of 6-piperidino-5,6-dihydro-4-oxo-4H-pyrrolo[1,2-a]thieno -[2,3-f][1,4]diazepine in 120 ml of methanol, and the reaction mixture is stirred at room temperature for 15 minutes and then heated to reflux for 30 minutes. The methanol is then removed under vacuum and the solid residue ground in 200 ml of water. The precipitate is drained, washed with water, dried and recrystallized. 1.2 g of 5,6-dihydro-4-oxo-4H-pyrrolo[1,2-a]-thieno[2,3-f][1,4]diazepine are obtained in the form of white crystals, melting point 191° C. (ethyl ether).

후처리

  1. temperatureheated
  2. temperatureto reflux for 30 minutes
  3. customThe methanol is then removed under vacuum
  4. washwashed with water
  5. customdried
  6. customrecrystallized

출처 및 근거

ORD 기록
ord-154e5f38feab4a70918056aafaab89d6
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05130301

반응 노트

불러오는 중…