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Ammonia → 2-(2,2-Dimethylpropyl)-2-hydroxymethylpropane-1,3-diol

HRID 345374
ノート
印刷プレビュー

反応式

HRID 345374 の反応式
C([O:8][CH2:9][C:10]([CH2:15][C:16]([CH3:19])([CH3:18])[CH3:17])([CH2:13][OH:14])[CH2:11][OH:12])C1C=CC=CC=1.N.[Na].[Cl-].[NH4+]>C(OCC)C>[CH3:17][C:16]([CH3:19])([CH3:18])[CH2:15][C:10]([CH2:9][OH:8])([CH2:13][OH:14])[CH2:11][OH:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 25517Ammonium ChlorideHCID 5360545SodiumHCID 150219552-Benzyloxymethyl-2-(2,2-dimethylpropyl)-propan-1,3-diol

生成物 1

HCID 189533432-(2,2-Dimethylpropyl)-2-hydroxymethylpropane-1,3-diol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

2-Benzyloxymethyl-2-(2,2-dimethylpropyl)-propan-1,3-diol (5.5 g.) in dry diethyl ether (50 ml.) was added to liquid ammonia (200 ml.) at -70°. Sodium (2.5 g.) was added to the stirred solution. Stirring was maintained at -70°, for 1 hour. The mixture was allowed to warm up to -30° and solid ammonium chloride (15 g.) was added cautiously. The ammonia was removed from the reaction mixture under a current of nitrogen. Methanol (25 ml.) was added to the stirred mixture to destroy residual sodium. Dichloromethane (400 ml.) was added and the mixture was filtered. The filtrates were evaporated in vacuo. 2-(2,2-Dimethylpropyl)-2-hydroxymethyl-propan-1,3-diol was obtained as a colourless solid (3.5 g.).

後処理

  1. temperaturewas maintained at -70°, for 1 hour
  2. temperatureto warm up to -30°
  3. customThe ammonia was removed from the reaction mixture under a current of nitrogen
  4. additionMethanol (25 ml.) was added to the stirred mixture
  5. customto destroy residual sodium
  6. additionDichloromethane (400 ml.) was added
  7. filtrationthe mixture was filtered
  8. customThe filtrates were evaporated in vacuo

出典と根拠

ORDレコード
ord-b64b097149c64398b28302d50e86a104
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05057508

反応ノート

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