Benzyl chloroformate → 3-(((Benzyloxy)carbonyl)amino)-2-methylpropanoic acid

HRID 973780

반응식

HRID 973780 반응식
[NH2:1][CH2:2][CH:3]([CH3:7])[C:4]([OH:6])=[O:5].[CH2:8]([O:15][C:16](Cl)=[O:17])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>N1C=CC=CC=1.O>[C:16]([NH:1][CH2:2][CH:3]([CH3:7])[C:4]([OH:6])=[O:5])([O:15][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:17]

참가 물질

5

반응 조건

온도
0 °C

실험 절차

In a mixture of 10 ml of pyridine and 10 ml of water was dissolved 500 mg of β-amino-isobutyric acid, and 1.5 ml of benzyloxycarbonyl chloride was dropped thereinto with stirring at 0° C. After completion of the dropping, the resulting mixture was stirring of room temperature for 3 hours, after which the pyridine was removed under reduced pressure. Then, hydrochloric acid was added to the residue, and the resulting mixture was extracted with ethyl acetate. The ethyl acetate layer obtained was washed successively with diluted hydrochloric acid, water and an aqueous sodium chloride solution, and then concentrated to obtain an oily substance. Subsequently, the oily substance was washed with a mixed solvent of ether and hexane to obtain 380 mg of the desired compound.

후처리

  1. additionwas dropped
  2. stirringAfter completion of the dropping, the resulting mixture was stirring of room temperature for 3 hours
  3. customafter which the pyridine was removed under reduced pressure
  4. additionThen, hydrochloric acid was added to the residue
  5. extractionthe resulting mixture was extracted with ethyl acetate
  6. customThe ethyl acetate layer obtained
  7. washwas washed successively with diluted hydrochloric acid, water
  8. concentrationan aqueous sodium chloride solution, and then concentrated
  9. customto obtain an oily substance
  10. washSubsequently, the oily substance was washed with a mixed solvent of ether and hexane

출처 및 근거

ORD 기록
ord-14531f34701b4a69bc63b6f70e00a2a5
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05064945

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