Potassium Carbonate → HCID 20309567、化合物

HRID 972795ノート

反応式

HRID 972795 の反応式
[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]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 18430EpibromohydrinHCID 20309539HCID 20309539、化合物

生成物 1

HCID 20309567HCID 20309567、化合物収率 57.8%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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°).

後処理

  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

出典と根拠

ORDレコード
ord-5f1724c00f9f470f82941ac178734acc
出典データセット
uspto-grants-1977_10
特許番号
US04053601

反応ノート

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