Ethyl Acetate → N-(2-chloro-5-nitrophenyl)-4-methylbenzamide

HRID 1886942노트

반응식

HRID 1886942 반응식
[Cl:1][C:2]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=1[NH2:4].[CH3:12][C:13]1[CH:21]=[CH:20][C:16]([C:17](Cl)=[O:18])=[CH:15][CH:14]=1.C(OCC)(=O)C>N1C=CC=CC=1>[Cl:1][C:2]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=1[NH:4][C:17](=[O:18])[C:16]1[CH:20]=[CH:21][C:13]([CH3:12])=[CH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 134054-Methylbenzoyl ChlorideHCID 226912-Chloro-5-nitroaniline

생성물 1

HCID 3330399N-(2-chloro-5-nitrophenyl)-4-methylbenzamide수율 42%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

To 2-chloro-5-nitroaniline (2 g, 11.59 mmol) in pyridine (5 mL) at room temperature was added 4-methylbenzoyl chloride (1.6 mL, 12.17 mmol), followed by pyridine (5 mL). The mixture was then stirred at room temperature for 16 h. Ethyl acetate was then added to the solution to give a precipitate, which was filtered off and washed twice with ethyl acetate, and then hexanes. The resulting solid was then washed with aqueous sodium bicarbonate, 1M aqueous sodium hydroxide, water and hexanes to afford (1.4 g, 42%) of the title compound.

후처리

  1. customto give a precipitate, which
  2. filtrationwas filtered off
  3. washwashed twice with ethyl acetate
  4. washThe resulting solid was then washed with aqueous sodium bicarbonate, 1M aqueous sodium hydroxide, water and hexanes

출처 및 근거

ORD 기록
ord-6bb81c9d3b6c43758f0afe627ec5bcc0
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501713B2

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