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Ammonium Hydroxide → 3-Nitro-5-(trifluoromethyl)benzamide

HRID 1050186
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HRID 1050186 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:12]=1)[C:7](Cl)=[O:8])([O-:3])=[O:2].[NH4+:17].[OH-]>C1COCC1>[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:12]=1)[C:7]([NH2:17])=[O:8])([O-:3])=[O:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 226083993-Nitro-5-(trifluoromethyl)benzoyl chloride

생성물 1

HCID 105376213-Nitro-5-(trifluoromethyl)benzamide수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
20 °C

실험 절차

To a mixture of 3-nitro-5-(trifluoromethyl)benzoyl chloride (1.8 g, 7.10 mmol) in THF (20 mL) was added NH4OH (2.96 mL, 21.30 mmol) at 20° C. The mixture was stirred at 20° C. for 12 h. LCMS showed the reaction was finished. The mixture was extracted with EA, washed with water, and concentrated to give 3-nitro-5-(trifluoromethyl)benzamide (1.5 g, 5.86 mmol, 83% yield): 1H NMR (400 MHz, DMSO-d6) δ 8.91 (s, 1H), 8.62 (br.s, 2H), 8.53 (s, 1H), 7.93 (s., 1H). ES-LCMS m/z 235 (M+H).

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후처리

  1. extractionThe mixture was extracted with EA
  2. washwashed with water
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-53c203ec4ecf486d951832bd5bac4197
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382238B2

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