3-[(4-Chlorophenyl)thio]pentane-2,4-dione → HCID 22174886、化合物
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:12]=[CH:11][N:10]=[C:9]([NH:13][NH2:14])[N:8]=1.[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([S:22][CH:23]([C:27](=O)[CH3:28])[C:24](=O)[CH3:25])=[CH:18][CH:17]=1>C(O)CC>[Cl:15][C:16]1[CH:17]=[CH:18][C:19]([S:22][C:23]2[C:24]([CH3:25])=[N:14][N:13]([C:9]3[N:8]=[C:7]([C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=4)[N:12]=[CH:11][N:10]=3)[C:27]=2[CH3:28])=[CH:20][CH:21]=1参加物
4
反応条件
- 温度
- 95 °C
実験手順
A stirred suspension of the product of step 3 (0.333 g, 1.77 mmol) and 3-(4-chloro-phenylsulfanyl)-pentane-2,4-dione (0.473 g, 1.95 mmol) in n-propanol was heated at 95° C. overnight. The reaction solution was concentrated directly onto silica and flash chromatographed (methylene chloride/methanol) to afford a dirty yellow solid. This material was further purified by trituration with diethyl ether to afford 0.056 g (8%) of product as a white solid: 1H NMR (DMSO-d6) δ 9.44 (s, 1H), 8.94-8.77 (m, 1H), 8.68-8.43 (m, 1H), 8.18-7.96 (m, 1H), 7.77-7.57 (m, 1H), 7.45-7.24 (m, 2H), 7.20-6.98 (m, 2H), 2.83 (s, 3H), 2.20 (s, 3H) ppm.