Epibromohydrin → HCID 20309567, 화합물

HRID 1579286노트

반응식

HRID 1579286 반응식
[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([OH:19])=[C:9]([CH:18]=1)[C:10]([CH2:12][CH2:13][C:14]([O:16][CH3:17])=[O:15])=[O:11])(=[O:3])[CH3:2].[CH2:20]([CH:22]1[O:24][CH2:23]1)Br>C(C(C)=O)C>[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([O:19][CH2:20][CH:22]2[O:24][CH2:23]2)=[C:9]([CH:18]=1)[C:10]([CH2:12][CH2:13][C:14]([O:16][CH3:17])=[O:15])=[O:11])(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 18430EpibromohydrinHCID 20309539HCID 20309539, 화합물

생성물 1

HCID 20309567HCID 20309567, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

Methyl 3-(5-acetamido-2-hydroxybenzoyl)propionate (0.75 g) anhydrous potassium carbonate (0.39 g), epibromohydrin (0.78 g) and dry methyl ethyl ketone (20 ml) were stirred and heated under reflux for 16 hours. The cooled reaction mixture was filtered, the filtrate evaporated under reduced pressure and the residual oil purified by elution from a silica column with chloroform/methanol. Methyl 3-[5-acetamido-2-(2,3-epoxypropoxy)benzoyl]propionate was obtained as an oil which solidified, (0.52 g, 57%, m.p. 84°-87°C; M+, 321, M 321).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 16 hours
  3. customThe cooled reaction mixture
  4. filtrationwas filtered
  5. customthe filtrate evaporated under reduced pressure
  6. customthe residual oil purified by elution from a silica column with chloroform/methanol

출처 및 근거

ORD 기록
ord-7784477ce8f943cab927b6069125a0df
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931177

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