Epibromohydrin → HCID 20309567, 화합물

HRID 596693노트

반응식

HRID 596693 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 (0.75g) anhydrous potassium carbonate (0.39g), epibromohydrin (0.78g) 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, (0.52g, 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-e85a9f23b1cc4588bbf96612d8ac5f97
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04011321

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