1-Cyclopropylpiperazine → HCID 67325292、化合物
反応式
[F:1][CH:2]([F:14])[O:3][C:4]1[CH:9]=[C:8](F)[CH:7]=[CH:6][C:5]=1[N+:11]([O-:13])=[O:12].[CH:15]1([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[CH2:17][CH2:16]1>C(#N)C>[CH:15]1([N:18]2[CH2:23][CH2:22][N:21]([C:8]3[CH:7]=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[C:4]([O:3][CH:2]([F:14])[F:1])[CH:9]=3)[CH2:20][CH2:19]2)[CH2:17][CH2:16]1参加物
4
反応条件
- 温度
- 100 °C
実験手順
To 2.07 g (10.0 mmol) of the product prepared in step 14.1 in 30 mL of acetonitrile are added 5.99 mL (35.0 mmol) of diispropylethylamine and then 2.09 g (10.5 mmol) of finely ground N-cyclopropylpiperazine (supplier). The reaction mixture is heated at 100°C. for 1 hour 30 minutes, cooled and concentrated under vacuum. The residue is taken up in 75 mL of ethyl acetate and washed with saturated aqueous NaHCO3 solution and with saturated aqueous NaCl solution. The organic phase is dried over Na2SO4, filtered and concentrated under vacuum. After triturating in cyclohexane, the solid is drained by suction and dried in an oven under vacuum. 2.33 g of the expected product are obtained in the form of a yellow solid, which is used as obtained in the following step. Yield=74.5%.