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

HRID 264958

반응식

HRID 264958 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 1140Toluene용매HCID 14798Sodium Hydroxide용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-479d9b550e9a4bdfb9e5eb8ca5818ecf
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646143

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