Methanol → HCID 12069505, 화합물

HRID 398517노트

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HRID 398517 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9](N)=[O:10])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[CH3:15][OH:16]>>[CH3:15][O:16][C:9](=[O:10])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([N+:12]([O-:14])=[O:13])[CH:4]=1

참가 물질

3

반응물 2

HCID 887MethanolHCID 5216164-Chloro-3-nitrophenylacetamide

생성물 1

HCID 12069505HCID 12069505, 화합물수율 89%

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온도
25 °C

실험 절차

A solution of 4-chloro-3-nitrophenylacetamide (2.00 g, 9.32 mmol) in methanol (40 mL) was treated with Amberlyst® 15 ion exchange resin (15.00 g). The resulting reaction mixture was heated under reflux for 64 h. The reaction mixture was allowed to cool to 25° C. and then filtered to remove the Amberlyst® 15 ion exchange resin. The filtrate was concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230-400 mesh, 3/1 hexanes/ethyl acetate) afforded 4-chloro-3-nitro-phenylacetic acid methyl ester (1.91 g, 89%) as a yellow oil: EI-HRMS m/e calcd for C9H8ClNO4 (M+) 229.0142, found 229.0146.

후처리

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureunder reflux for 64 h
  4. filtrationfiltered
  5. customto remove the Amberlyst® 15 ion exchange resin
  6. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-379f602795cb4170a2d407e6f41f3a19
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610846B1

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