Potassium Carbonate → HCID 20309567, 화합물

HRID 972795노트

반응식

HRID 972795 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].C(=O)([O-])[O-].[K+].[K+].[CH2:26]([CH:28]1[O:30][CH2:29]1)Br>CC(CC)=O>[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]([O:19][CH2:26][CH:28]2[O:30][CH2:29]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

5

반응물 3

HCID 11430Potassium CarbonateHCID 18430EpibromohydrinHCID 20309539HCID 20309539, 화합물

생성물 1

HCID 20309567HCID 20309567, 화합물수율 57.8%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

Methyl 3-(5-acetamido-2-hydroxybenzoyl)propionate (0.75 g, 0.0028 mole), anhydrous potassium carbonate (0.39 g, 0.0028 mole), epibromohydrin (0.78 g, 0.00565 mole) and dry ethyl methyl ketone (20 ml) were stirred and heated under reflux for 16 hours. The cooled mixture was filtered and evaporated under reduced pressure to an oil which was purified by elution from a silica column with chloroformmethanol to give methyl 3-[5-acetamido-2-(2,3-epoxypropoxy)benzoyl]propionate (0.52 g, 57%, m.p. 84°-87°).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 16 hours
  3. filtrationThe cooled mixture was filtered
  4. customevaporated under reduced pressure to an oil which
  5. customwas purified by elution from a silica column with chloroformmethanol

출처 및 근거

ORD 기록
ord-5f1724c00f9f470f82941ac178734acc
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04053601

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