Epibromohydrin → HCID 20309567、化合物

HRID 596693ノート

反応式

HRID 596693 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].[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]

参加物

4

反応物 2

HCID 18430EpibromohydrinHCID 20309539HCID 20309539、化合物

生成物 1

HCID 20309567HCID 20309567、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

Methyl 3-(5-acetamido-2-hydroxybenzoyl)propionate (0.75g) 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).

後処理

  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

出典と根拠

ORDレコード
ord-e85a9f23b1cc4588bbf96612d8ac5f97
出典データセット
uspto-grants-1977_03
特許番号
US04011321

反応ノート

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