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2-Nitrobenzoyl chloride → N-[4-bromo-3-(trifluoromethyl)phenyl]-2-nitrobenzamide

HRID 8897
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HRID 8897 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]([F:12])([F:11])[F:10])[C:5]([Br:8])=[CH:6][CH:7]=1.[OH-].[Na+].[N+:15]([C:18]1[CH:26]=[CH:25][CH:24]=[CH:23][C:19]=1[C:20](Cl)=[O:21])([O-:17])=[O:16]>C(OCC)(=O)C>[N+:15]([C:18]1[CH:26]=[CH:25][CH:24]=[CH:23][C:19]=1[C:20]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[C:4]([C:9]([F:12])([F:10])[F:11])[CH:3]=1)=[O:21])([O-:17])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 118752-Nitrobenzoyl chlorideHCID 14798Sodium HydroxideHCID 678524-Bromo-3-(trifluoromethyl)aniline

생성물 1

HCID 1300995N-[4-bromo-3-(trifluoromethyl)phenyl]-2-nitrobenzamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 3-amino-6-bromobenzotrifluoride (Fluka, Buchs, Switzerland; 24.0 g, 100 mmol) in ethyl acetate (240 mL) is added to a stirred aqueous solution of sodium hydroxide (110 mL of 1 M) at room temperature. This stirred solution is then treated dropwise over 30 minutes with a solution of 2-nitrobenzoyl chloride (Fluka, Buchs, Switzerland; 14.5 mL, 110 mmol) in ethyl acetate (150 mL). The resulting mixture is then stirred for 30 min at ambient temperature. The mixture is extracted with ethyl acetate (3×100 mL) and the combined extracts are sequentially washed with hydrochloric acid (2×100 mL of 2M), water (2×100 mL), saturated aqueous sodium hydrogen carbonate solution (2×100 mL) and saturated aqueous sodium chloride (1×100 mL), dried (MgSO4), filtered and the solvent is evaporated under reduced pressure to yield the crude product which is purified by recrystallisation from ethyl acetate-hexane to give the title compound as a beige crystalline solid, m.p. 157–158° C.

후처리

  1. extractionThe mixture is extracted with ethyl acetate (3×100 mL)
  2. washthe combined extracts are sequentially washed with hydrochloric acid (2×100 mL of 2M), water (2×100 mL), saturated aqueous sodium hydrogen carbonate solution (2×100 mL) and saturated aqueous sodium chloride (1×100 mL)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent is evaporated under reduced pressure
  6. customto yield the crude product which
  7. customis purified by recrystallisation from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-08f8d6788814465f87faa5aa3662b783
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091224B2

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