Dichloromethane → HCID 86742082、化合物

反応式

Cl.[F:2][C:3]([F:25])([F:24])[C:4]1[CH:13]=[C:12]2[C:7]([C:8]([NH:14][C:15]3[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=3)=[CH:9][CH:10]=[N:11]2)=[CH:6][CH:5]=1.Cl.[N:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[S:33](C1CCNCC1)=[O:34].C([N:43]([CH2:46][CH3:47])[CH2:44][CH3:45])C.[CH2:48](Cl)Cl>>[N:43]1[CH:44]=[CH:45][CH:48]=[CH:47][C:46]=1[CH:29]1[CH2:30][CH2:31][CH2:32][N:27]([C:19](=[O:20])[C:18]2[CH:22]=[CH:23][C:15]([NH:14][C:8]3[C:7]4[C:12](=[CH:13][C:4]([C:3]([F:25])([F:24])[F:2])=[CH:5][CH:6]=4)[N:11]=[CH:10][CH:9]=3)=[CH:16][CH:17]=2)[C:28]1=[S:33]=[O:34]

参加物

反応物 4

HCID 6344Dichloromethane

HCID 8471Triethylamine

HCID 13603946HCID 13603946、化合物

HCID 13825050HCID 13825050、化合物

生成物 1

HCID 86742082HCID 86742082、化合物

実験手順

4-[[7-(Trifluoromethyl)-4-quinolyl]amino]benzoyl chloride hydrochloride (0.69 g) was added slowly to a stirred mixture of 4-[(2-pyridyl)sulfinyl]piperidine hydrochloride (0.50 g) and triethylamine (1.72 ml) in dry methylene chloride (22 ml) at room temperature. The resultant mixture was stirred at the same temperature for 1.5 hours and concentrated in vacuo. The residue was partitioned between chloroform and water. The organic layer was washed with saturated aqueous sodium bicarbonate, dried over magnesium sulfate, and concentrated to dryness in vacuo. The resultant crystalline residue was recrystallized from a mixture of methylene chloride and methanol and washed successively with methanol and methylene chloride to give 4-[(2-pyridyl(sulfinyl]-1-[4-[[7-(trifluoromethyl)-4-quinolyl]amino]benzoyl]piperidine (0.59 g).