Ethyl 4-bromo-3-oxobutanoate → HCID 178472904, 화합물

HRID 261671

반응식

HRID 261671 반응식
[N:1]([O-:3])=O.[Na+].[Br:5][CH2:6][C:7](=[O:14])[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]>O.C(O)(=O)C>[OH:3][N:1]=[C:8]([C:7]([CH2:6][Br:5])=[O:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10]

참가 물질

5

반응물 2

HCID 575284Ethyl 4-bromo-3-oxobutanoateHCID 23668193Sodium Nitrite

생성물 1

HCID 178472904HCID 178472904, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

반응 조건

온도
10 °C

실험 절차

A solution of sodium nitrite (12.4 g.) in water (150 ml.) was dropwise added with stirring at 5° to 7° C. to a solution of ethyl 4-bromoacetoacetate (30 g.) in acetic acid (200 ml.) and the mixture was stirred for 2 hours at 10° C. Water (200 ml.) was added to the reaction mixture and the resultant mixture was extracted with ether (500 ml.). The extract was washed twice with water (200 ml.) and with a sodium chloride aqueous solution (200 ml.) and dried over magnesium sulfate. The solvent was distilled off under reduced pressure to give yellowish brown crystals of ethyl 2-hydroxyimino-4-bromoacetoacetate (a mixture of syn and anti isomers) (32.6 g.).

후처리

  1. extractionthe resultant mixture was extracted with ether (500 ml.)
  2. washThe extract was washed twice with water (200 ml.) and with a sodium chloride aqueous solution (200 ml.)
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-d45a7d3ae8ca443dbb7fd8db381bb342
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166115

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