Dimethylformamide → HCID 20366149、化合物

反応式

[C:1]([C:3]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][C:9]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:12]([OH:14])=[O:13])[CH2:8][CH2:7]1)#[N:2].CN(C)C=O.[Cl:38][CH2:39][C:40]#[N:41].C(N(CC)CC)C>O>[ClH:38].[C:1]([C:3]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][C:9]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)([C:12]([O:14][CH2:39][C:40]#[N:41])=[O:13])[CH2:8][CH2:7]1)#[N:2]

参加物

実験手順

2.12 Grams of 1-(3-cyano-3,3-diphenylpropyl)-4-phenylpiperidine-4-carboxylic acid was dissolved in 60 ml. of redistilled N,N-dimethylformamide by warming to approximately 60° C. To the resultant solution was added .4 gram of chloracetonitrile, followed by .55 gram of triethylamine. The solution was stirred at room temperature under anhydrous conditions for about 24 hours, then diluted with water and extracted with ethyl acetate. The ethyl acetate extract was washed with water, acidified with concentrated hydrochloric acid in 2-propanol, diluted with ethyl ether and cooled. The precipitate which formed was recrystallized from a mixture of methanol and tetrahydrofuran, affording cyanomethyl 1-(3-cyano-3,3-diphenylpropyl)-4-phenylpiperidine-4-carboxylate hydrochloride, melting at about 243.5°-245.5° C.