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 1828251ノート

反応式

HRID 1828251 の反応式
[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

参加物

5

反応物 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

生成物 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-dioxide収率 86.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9893aebd9036475b9a9b6deb1ee982d2
出典データセット
uspto-grants-2006_06
特許番号
US07057036B2

反応ノート

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