Water → 2-[3-[4-(4-fluorophenyl)piperazin-1-yl]propyl]-5-hydroxy-7-methyl-3,4,5,7-tetrahydro-2H-pyrrolo[3,4-f][1,2]thiazepine 1,1-dioxide

HRID 649768노트

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HRID 649768 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[CH2:23][CH2:22][C:21](=[O:24])[C:20]4=[CH:25][N:26]([CH3:28])[CH:27]=[C:19]4[S:18]3(=[O:30])=[O:29])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[BH4-].[Na+].O>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[CH2:23][CH2:22][CH:21]([OH:24])[C:20]4=[CH:25][N:26]([CH3:28])[CH:27]=[C:19]4[S:18]3(=[O:30])=[O:29])[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 99107952-[3-[4-(4-fluorophenyl)piperazin-1-yl]propyl]-7-methyl-3,4,5,7-tetrahydro-2H-pyrrolo[3,4-f][1,2]thiazepin-5-one 1,1-dioxide

생성물 1

HCID 98030822-[3-[4-(4-fluorophenyl)piperazin-1-yl]propyl]-5-hydroxy-7-methyl-3,4,5,7-tetrahydro-2H-pyrrolo[3,4-f][1,2]thiazepine 1,1-dioxide수율 86.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of 174 mg (0.4 mmol) of Compound 24 in 8 ml of ethanol, 151 mg (4 mmol) of sodium borohydride were added gradually under ice-cooled stirring. The resulting mixture was stirred under ice cooling for 1 hour and further at room temperature for 13 hours. Water (80 ml) was added to the reaction mixture. The thus-obtained mixture was stirred at room temperature for 30 minutes and then concentrated under reduced pressure. Post treatment and purification were conducted as in Example 15, whereby 151 mg of the title compound were obtained (yield: 86%).

후처리

  1. additionwere added gradually under ice-
  2. temperaturecooled
  3. stirringThe resulting mixture was stirred under ice cooling for 1 hour and further at room temperature for 13 hours
  4. stirringThe thus-obtained mixture was stirred at room temperature for 30 minutes
  5. concentrationconcentrated under reduced pressure
  6. customPost treatment and purification

출처 및 근거

ORD 기록
ord-004e74c83e8040a29b3ddbd9f958956e
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271223B1

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