Benzyl chloroformate → Ethyl 3-(((benzyloxy)carbonyl)amino)-2,2-dimethylpropanoate

HRID 264952노트

반응식

HRID 264952 반응식
[CH2:1]([O:8][C:9](Cl)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:12]([O:14][C:15](=[O:21])[C:16]([CH3:20])([CH3:19])[CH2:17][NH2:18])[CH3:13]>C(OCC)(=O)C.C(=O)([O-])O.[Na+]>[CH2:12]([O:14][C:15](=[O:21])[C:16]([CH3:20])([CH3:19])[CH2:17][NH:18][C:9]([O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:10])[CH3:13]

참가 물질

5

반응물 2

HCID 10387Benzyl chloroformateHCID 421529Ethyl 3-amino-2,2-dimethylpropanoate

생성물 1

HCID 22364460Ethyl 3-(((benzyloxy)carbonyl)amino)-2,2-dimethylpropanoate

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

31 ml of 90% chloroformic acid benzyl ester are slowly added, at 0°-5° C., to 29.04 g of 3-amino-2,2-dimethylpropionic acid ethyl ester in 500 ml of ethyl acetate and 250 ml of 1M sodium hydrogen carbonate solution. The reaction mixture is stirred for 2 hours at 0°-5° C. and extracted with ethyl acetate. The organic phases are washed with saturated sodium chloride solution and then concentrated. The evaporation residue is purified by FC (1 kg of silica gel; eluant: ethyl acetate/hexane=1:3). The title compound is obtained: Rf (ethyl acetate/hexane=1:3)=0.28.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic phases are washed with saturated sodium chloride solution
  3. concentrationconcentrated
  4. customThe evaporation residue is purified by FC (1 kg of silica gel; eluant: ethyl acetate/hexane=1:3)

출처 및 근거

ORD 기록
ord-37bcdd1329554382ac4b7b0debfaebbf
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646143

반응 노트

불러오는 중…