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

HRID 400510ノート

反応式

HRID 400510 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 31374Dimethylacetamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-da3c75eb16554233b273b4d185c5c602
出典データセット
uspto-grants-2014_06
特許番号
US08741899B2

反応ノート

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