Acetic acid, 2-chloro-, phenylmethyl ester → Tert-butyl 2-benzyloxycarbonylmethoxyimino-3-oxobutyrate

HRID 569362

반응식

HRID 569362 반응식
[OH:1][N:2]=[C:3]([C:11](=[O:13])[CH3:12])[C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:21][C:22]([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23]>C(OCC)(=O)C.CN(C)C=O>[CH2:25]([O:24][C:22]([CH2:21][O:1][N:2]=[C:3]([C:11](=[O:13])[CH3:12])[C:4]([O:6][C:7]([CH3:9])([CH3:8])[CH3:10])=[O:5])=[O:23])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

참가 물질

6

반응물 3

HCID 8786Acetic acid, 2-chloro-, phenylmethyl esterHCID 11430Potassium CarbonateHCID 178468384tert-butyl 2-hydroxyimino-3-oxobutanoate

생성물 1

HCID 53811665Tert-butyl 2-benzyloxycarbonylmethoxyimino-3-oxobutyrate수율 95.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
40 °C

실험 절차

To a suspension of tert-butyl 2-hydroxyimino-3-oxobutyrate (56.4 g) and potassium carbonate (62.4 g) in ethyl acetate (300 ml) and N,N-dimethylformamide (60 ml) was added benzyl chloroacetate (60 g), and the mixture was stirred at 40° C. for 7 hours. The reaction mixture was poured into ice-water (1000 ml), and the separated organic layer was washed twice with a saturated aqueous solution of sodium chloride and then dried over magnesium sulfate. Removal of the solvent gave tert-butyl 2-benzyloxycarbonylmethoxyimino-3-oxobutyrate (96.3 g) as an oil.

후처리

  1. washthe separated organic layer was washed twice with a saturated aqueous solution of sodium chloride
  2. dry with materialdried over magnesium sulfate
  3. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-3228b8bd8b25419a9f5eca11a38f91e4
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731443

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