2-(4-Chlorophenyl)ethanethioamide → HCID 69448752、化合物
反応式
Br[CH2:2][C:3]([CH:5]1[CH2:10][CH2:9][N:8]([C:11]([O:13][CH2:14][CH:15]=[CH2:16])=[O:12])[CH2:7][CH2:6]1)=O.[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:24][C:25](=[S:27])[NH2:26])=[CH:20][CH:19]=1>C(O)C>[Cl:17][C:18]1[CH:19]=[CH:20][C:21]([CH2:24][C:25]2[S:27][CH:2]=[C:3]([CH:5]3[CH2:10][CH2:9][N:8]([C:11]([O:13][CH2:14][CH:15]=[CH2:16])=[O:12])[CH2:7][CH2:6]3)[N:26]=2)=[CH:22][CH:23]=1参加物
4
実験手順
A mixture of allyl 4-(bromoacetyl)piperidine-1-carboxylate (547 mg) and 2-(4-chlorophenyl)ethanethioamide (366 mg) in ethanol (15 ml) was refluxed for 5 hours. The reaction mixture was evaporated to dryness and the residue was purified by chromatography on silica eluting with methanol/dichloromethane (2:98) to give allyl 4-[2-(4-chlorobenzyl)-1,3-thiazol-4-yl]piperidine-1-carboxylate. Yield 698 mg. NMR (CDCl3): 1.65 (m, 2H), 2.25 (m, 2H), 2.95 (m, 2H), 3.2 (m, 1H), 4.3 (m, 2H), 4.55 (m, 4H), 5.3 (m, 2H), 6.0 (m, 1H), 6.95 (s, 1H), 7.35 (m, 4H).
後処理
- temperaturewas refluxed for 5 hours
- customThe reaction mixture was evaporated to dryness
- customthe residue was purified by chromatography on silica eluting with methanol/dichloromethane (2:98)
出典と根拠
- ORDレコード
- ord-09d090415d694169962be4fb7eaf3062
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07294636B2
反応ノート
読み込み中…