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

HRID 654064ノート

反応式

HRID 654064 の反応式
[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

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 10850843HCID 10850843、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-154e5f38feab4a70918056aafaab89d6
出典データセット
uspto-grants-1992_07
特許番号
US05130301

反応ノート

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