HCID 178474037、化合物 → HCID 20186463、化合物

HRID 2308953ノート

反応式

HRID 2308953 の反応式
[C:1]([NH:4][C:5]1[CH:6]=[CH:7][C:8]2[C:9]([C:12](=[O:20])[C:13]([CH2:16][C:17]([OH:19])=[O:18])=[CH:14][CH:15]=2)=[CH:10][CH:11]=1)(=[O:3])[CH3:2]>C(O)(=O)C.[Zn]>[C:1]([NH:4][CH:5]1[CH2:11][CH2:10][C:9]2[C:12](=[O:20])[CH:13]([CH2:16][C:17]([OH:19])=[O:18])[CH:14]=[CH:15][C:8]=2[CH2:7][CH2:6]1)(=[O:3])[CH3:2]

参加物

4

反応物 1

HCID 178474037HCID 178474037、化合物

生成物 1

HCID 20186463HCID 20186463、化合物収率 83.1%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

Zinc dust (5.3 g) is added in portions to a stirred suspension of the 7-acetylamino-1-oxo-benzocyclohepten-2-yl-acetic acid (6 g) in 80% aqueous acetic acid (70 ml), warmed at 100° C.; the stirring is continued for 1 hour. The inorganic materials are removed by filtration and washed with warm 80% aqueous acetic acid (70 ml).The eluates are collected and acetic acid is distilled off under vacuum. The residual aqueous phase is extracted with ethyl ether, the combined extracts are dried on Na2SO4 and the solvents are evaporated. The crude material is triturated with hexane-ethyl ether to give 7-acetylamino-1-oxo-benzocycloheptan-2-yl-acetic acid (5.1 g) m.p. 198° C.

後処理

  1. customThe inorganic materials are removed by filtration
  2. washwashed
  3. temperaturewith warm 80% aqueous acetic acid (70 ml).The eluates
  4. customare collected
  5. distillationacetic acid is distilled off under vacuum
  6. extractionThe residual aqueous phase is extracted with ethyl ether
  7. customthe combined extracts are dried on Na2SO4
  8. customthe solvents are evaporated
  9. customThe crude material is triturated with hexane-ethyl ether

出典と根拠

ORDレコード
ord-e43ea65b60fc4d45b64288058c54ed3a
出典データセット
uspto-grants-1987_09
特許番号
US04692447

反応ノート

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