2-Bromoethanol → HCID 86629018、化合物

HRID 1013437ノート

反応式

HRID 1013437 の反応式
[NH2:1][C@H:2]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:3][C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5].Br[CH2:19][CH2:20][OH:21].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[OH:21][CH2:20][CH2:19][NH:1][C@@H:2]([CH2:3][C:4]([O:6][C:7]([CH3:9])([CH3:10])[CH3:8])=[O:5])[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12]

参加物

5

反応物 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 7269469D-aspartic acid di-t-butyl ester

生成物 1

HCID 86629018HCID 86629018、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of di-tert-butyl L-aspartate (5.62 g-20 mmol), 2-bromoethanol (2.84 ml-40 mmol) and K2CO3 (5.6 g-40 mmol) in 100 ml of acetonitrile is heated at reflux for 16 hours. The mineral salts are filtered off and the solvent is removed by distillation in vacuo. The crude product so obtained is purified by flash chromatography on silica gel using a (95/5) dichloromethane/ethanol mixture as eluant. The expected product is obtained in the form of a colourless oil.

後処理

  1. temperatureat reflux for 16 hours
  2. filtrationThe mineral salts are filtered off
  3. customthe solvent is removed by distillation in vacuo
  4. customThe crude product so obtained
  5. customis purified by flash chromatography on silica gel using a (95/5) dichloromethane/ethanol mixture as eluant

出典と根拠

ORDレコード
ord-3d01342a0d654d76a4bdc76d6348a218
出典データセット
uspto-grants-2011_07
特許番号
US07981920B2

反応ノート

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