HCID 178474037, 화합물 → HCID 20186463, 화합물

HRID 2308953노트

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HRID 2308953 반응식
[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]

참가 물질

4

반응물 1

HCID 178474037HCID 178474037, 화합물

생성물 1

HCID 20186463HCID 20186463, 화합물수율 83.1%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

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온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e43ea65b60fc4d45b64288058c54ed3a
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692447

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