Hydrochloric Acid → HCID 178479495、化合物
反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:25]=[CH:24][C:17]([C:18]([NH:20][C:21]([NH2:23])=[NH:22])=[O:19])=[CH:16][C:15]=2[C:26]([F:29])([F:28])[F:27])[CH2:10][CH2:9]1)=[O:7].[ClH:30]>O>[OH2:7].[ClH:30].[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[CH:25]=[CH:24][C:17]([C:18]([NH:20][C:21]([NH2:23])=[NH:22])=[O:19])=[CH:16][C:15]=2[C:26]([F:28])([F:29])[F:27])[CH2:12][CH2:13]1)=[O:7]参加物
4
反応条件
- 温度
- 50 °C
実験手順
109.4 g of 4-[4-(2-pyrrolylcarbonyl)-1-piperazinyl]-3-trifluoromethylbenzoylguanidine is suspended in 1.5 L of water and heated to about 50° C. 26.1 mL of concentrated aqueous hydrochloric acid is diluted with 300 mL of water and added dropwise to the preheated suspension within about 20 minutes. The mixture is stirred for about 15 minutes at constant temperature. Then the temperature is lowered to about 35° C. with stirring over a period of about 1.5 hours. It is then cooled to 5° C. to 10° C. and stirred for another hour at this temperature. The crystals obtained are separated off, washed with a little water, and dried in vacuo at about 50° C. Yield: 116.5 g; melting point: 180° C. ±5° C. (DSC at a heating rate of 10 K/min).