4-(Trifluoromethyl)aniline → Ethyl 3-({[4-(trifluoromethyl)phenyl]amino}sulfonyl)benzoate

HRID 400510노트

반응식

HRID 400510 반응식
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:13]=[CH:14][CH:15]=1)[C:8]([O:10][CH2:11][CH3:12])=[O:9])(=[O:4])=[O:3].[F:16][C:17]([F:26])([F:25])[C:18]1[CH:24]=[CH:23][C:21]([NH2:22])=[CH:20][CH:19]=1>CN(C)C(=O)C.C(OCC)(=O)C>[F:16][C:17]([F:25])([F:26])[C:18]1[CH:19]=[CH:20][C:21]([NH:22][S:2]([C:5]2[CH:6]=[C:7]([CH:13]=[CH:14][CH:15]=2)[C:8]([O:10][CH2:11][CH3:12])=[O:9])(=[O:4])=[O:3])=[CH:23][CH:24]=1

참가 물질

5

반응물 2

HCID 99644-(Trifluoromethyl)anilineHCID 19790734Ethyl 3-(chlorosulfonyl)benzoate

생성물 1

HCID 66675205Ethyl 3-({[4-(trifluoromethyl)phenyl]amino}sulfonyl)benzoate

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 31374Dimethylacetamide용매

실험 절차

To ethyl 3-(chlorosulfonyl)benzoate (4.0 g, 16.08 mmol) in N,N-dimethylacetamide (20 mL) was added 4-(trifluoromethyl)aniline (10.37 g, 64.3 mmol) dropwise at room temperature. The mixture was stirred at room temperature for 2.5 hours, and then it was diluted with ethyl acetate (130 mL). The organic solution was washed with 1 N HCl (2×60 mL) and saturated NaCl (60 mL). The organic layer was concentrated, ethanol (40 mL) was added, and the mixture was concentrated to give ethyl 3-({[4-(trifluoromethyl)phenyl]amino}sulfonyl)benzoate.

후처리

  1. washThe organic solution was washed with 1 N HCl (2×60 mL) and saturated NaCl (60 mL)
  2. concentrationThe organic layer was concentrated
  3. additionethanol (40 mL) was added
  4. concentrationthe mixture was concentrated

출처 및 근거

ORD 기록
ord-da3c75eb16554233b273b4d185c5c602
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741899B2

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