Sodium Hydroxide → 2-Benzylthiomethyl-2-isobutyl-propan-1,3-diol

HRID 704140ノート

反応式

HRID 704140 の反応式
[CH2:1]([S:8][CH2:9][C:10]([CH2:21][CH:22]([CH3:24])[CH3:23])([C:16](OCC)=[O:17])[C:11](OCC)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>C(OCC)C>[CH2:1]([S:8][CH2:9][C:10]([CH2:21][CH:22]([CH3:24])[CH3:23])([CH2:16][OH:17])[CH2:11][OH:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 20075597HCID 20075597、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 200755682-Benzylthiomethyl-2-isobutyl-propan-1,3-diol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

Diethyl 2-benzylthiomethyl-2-isobutylmalonate (32.0 g.) in dry diethyl ether (60 ml.) was added to a stirred suspension of lithium aluminium hydride (7.0 g.) in dry diethyl ether (400 ml.), at 0°, under nitrogen. The mixture was stirred at room temperature for three hours and then refluxed with stirring for a further three hours. The mixture was cooled and 10% aqueous sodium hydroxide solution (25 ml.) was added very carefully. The mixture was filtered and the solid was washed with ether. The filtrates were dried over anhydrous magnesium sulphate and evaporated in vacuo. 2-Benzylthiomethyl-2-isobutyl-propan-1,3-diol was obtained as a colourless solid (20 g.) and was used without further purification.

後処理

  1. temperaturerefluxed
  2. stirringwith stirring for a further three hours
  3. temperatureThe mixture was cooled
  4. filtrationThe mixture was filtered
  5. washthe solid was washed with ether
  6. dry with materialThe filtrates were dried over anhydrous magnesium sulphate
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-d42ee46465c7435fad122ec6bb222dc1
出典データセット
uspto-grants-1991_01
特許番号
US04985582

反応ノート

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