反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH:28]2[CH2:30][CH2:29]2)[S:15]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[CH:19]=2)(=[O:17])=[O:16])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N1CCC(NC2CC2)CC1)C1C=CC=CC=1.C(N(CC)CC)C.FC(F)(F)C1C=C(S(Cl)(=O)=O)C=CC=1.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH:28]1([N:14]([CH:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)[S:15]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:27])([F:25])[F:26])[CH:19]=2)(=[O:16])=[O:17])[CH2:30][CH2:29]1.[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH:28]2[CH2:30][CH2:29]2)[S:15]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:25])([F:27])[F:26])[CH:19]=2)(=[O:16])=[O:17])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
反応物 5
生成物 2
試薬・触媒・溶媒 1
実験手順
N-(1-Benzylpiperidin-4-yl)-N-cyclopropyl-3-trifluoromethyl-benzenesulfonamide: N-Benzyl-4-cyclopropylaminopiperidine (5.0 g, 21.71 mmol) and triethylamine (3.6 mL, 26.05 mmol) were dissolved in dichloromethane (DCM, 100 mL). 3-Trifluoromethylbenzenesulfonyl chloride (3.47 mL, 21.71 mmol) was added and the resulting reaction mixture was stirred overnight. The mixture then was poured into potassium carbonate solution (200 mL), extracted with ether (2×200 mL), dried (MgSO4), and concentrated in vacuum to give a crude product as a yellow gum, which was purified by column chromatography on silica gel (hexane/EtOAc, 2:1). The title compound N-(1-benzylpiperidin-4-yl)-N-cyclopropyl-3-trifluoromethyl-benzenesulfonamide was obtained (9 g, 95% yield) as a pale yellow gum. Rf=0.42 (UV detection).
後処理
- customthe resulting reaction mixture
- extractionextracted with ether (2×200 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuum
- customto give a crude product as a yellow gum, which
- customwas purified by column chromatography on silica gel (hexane/EtOAc, 2:1)
出典と根拠
- ORDレコード
- ord-1f6641ea8fe248938efe7100e90267a5
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08937181B2
関連ノート
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