2-Bromoethanol → HCID 86629018, 화합물

HRID 1013437노트

반응식

HRID 1013437 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 86629018HCID 86629018, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3d01342a0d654d76a4bdc76d6348a218
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981920B2

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