Diethyl Ether → 3-(((Benzyloxy)carbonyl)amino)-2-methylpropanoic acid

HRID 264958

反応式

HRID 264958 の反応式
[CH2:1]([O:8][C:9](Cl)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:12][CH2:13][CH:14]([CH3:18])[C:15]([OH:17])=[O:16].C(OCC)C>C1(C)C=CC=CC=1.[OH-].[Na+]>[CH2:1]([O:8][C:9]([NH:12][CH2:13][CH:14]([CH3:18])[C:15]([OH:17])=[O:16])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 10387Benzyl chloroformateHCID 64956Beta-Aminoisobutyric Acid

生成物 1

HCID 3042743-(((Benzyloxy)carbonyl)amino)-2-methylpropanoic acid

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 14798Sodium Hydroxide溶媒

反応条件

温度
0 °C

実験手順

A solution of 41.7 ml of chloroformic acid benzyl ester (90%) in toluene is added to 25 g of 3-amino-2(R,S)-methylpropionic acid in 533 ml of 1N sodium hydroxide at 0° C. The reaction mixture is then stirred for 30 minutes at 0° C. After the addition of 400 ml of diethyl ether, the aqueous phase is removed and 140 ml of 4N hydrochloric acid are added. The crude title compound is obtained from the organic phase by extraction with diethyl ether: Rf (dichloromethane/methanol=8:2)=0.41.

後処理

  1. customthe aqueous phase is removed
  2. addition140 ml of 4N hydrochloric acid are added

出典と根拠

ORDレコード
ord-479d9b550e9a4bdfb9e5eb8ca5818ecf
出典データセット
uspto-grants-1997_07
特許番号
US05646143

関連ノート

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