Water → N-(2-chloro-5-nitrophenyl)-3,4-dimethoxybenzamide

HRID 991418

반응식

HRID 991418 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[C:6](Cl)=[O:7].[Cl:14][C:15]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][C:16]=1[NH2:17].O>N1C=CC=CC=1>[Cl:14][C:15]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][C:16]=1[NH:17][C:6](=[O:7])[C:5]1[CH:9]=[CH:10][C:11]([O:12][CH3:13])=[C:3]([O:2][CH3:1])[CH:4]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 226912-Chloro-5-nitroanilineHCID 77070Veratroyl chloride

생성물 1

HCID 3551001N-(2-chloro-5-nitrophenyl)-3,4-dimethoxybenzamide수율 35.8%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
100 °C

실험 절차

3,4-Dimethoxybenzoyl chloride (2 g) was added to a stirred suspension of 2-chloro-5-nitroaniline (1.72 g) in pyridine (10 ml) at 20° C. The reaction mixture was heated to 100° C. for 1 hour. After cooling to ambient temperature, the reaction mixture was poured into water (100 ml). The resulting precipitate was collected, washed with water and dried. The solid was triturated under methylene chloride (20 ml) to give N-(2-chloro-5-nitrophenyl)-3,4-dimethoxybenzamide (1.2 g), m.p. 231-232° C.; NMR Spectrum: (DMSOd6) 3.82 (s, 6H), 7.08 (d, 1H), 7.62 (m, 1H), 7.82 (d, 1H), 8.08 (m, 1H), 8.54 (d, 1H), 10.07 (m, 1H);

후처리

  1. temperatureAfter cooling to ambient temperature
  2. customThe resulting precipitate was collected
  3. washwashed with water
  4. customdried
  5. customThe solid was triturated under methylene chloride (20 ml)

출처 및 근거

ORD 기록
ord-be5cac2653734e61a10a60d8b32c5330
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06465455B1

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