Epibromohydrin → HCID 20309567、化合物

HRID 1579286ノート

反応式

HRID 1579286 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 (0.75 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).

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-7784477ce8f943cab927b6069125a0df
出典データセット
uspto-grants-1976_01
特許番号
US03931177

反応ノート

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