Water → 4-(3-Chloropropylthio)benzylalcohol

HRID 867905ノート

反応式

HRID 867905 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][CH2:8][CH2:9][CH2:10][S:11][C:12]1[CH:21]=[CH:20][C:15]([C:16](OC)=[O:17])=[CH:14][CH:13]=1.O>O1CCCC1>[Cl:7][CH2:8][CH2:9][CH2:10][S:11][C:12]1[CH:13]=[CH:14][C:15]([CH2:16][OH:17])=[CH:20][CH:21]=1

参加物

5

反応物 3

HCID 962WaterHCID 13749599Methyl 4-(3-chloropropylthio)benzoateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 137496004-(3-Chloropropylthio)benzylalcohol収率 85.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

5 g of lithium aluminum hydride are suspended in 200 ml of tetrahydrofuran, and a solution of 31.9 g of methyl 4-(3-chloropropylthio)benzoate in 200 ml of tetrahydrofuran is added thereto at 5° to 15° C. The mixture is stirred at the same temperature for 45 minutes. Water is added to the mixture at a temperature of below 20° C., and insoluble materials are filtered off. The filtrate is concentrated under reduced pressure to remove solvent, and the residue is distilled under reduced pressure. 24.1 g of 4-(3-chloropropylthio)benzylalcohol are obtained as an oil. Yield: 85%.

後処理

  1. customat 5° to 15° C
  2. filtrationare filtered off
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. customto remove solvent
  5. distillationthe residue is distilled under reduced pressure

出典と根拠

ORDレコード
ord-4c65ace957d540199afe316b5fa277e2
出典データセット
uspto-grants-1988_10
特許番号
US04777178

反応ノート

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