2-Phenylglutaric anhydride → HCID 88678971、化合物
反応式
[NH2:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH:7]([NH:10][C:11]2[N:15]([CH2:16][C:17]3[O:18][CH:19]=[CH:20][CH:21]=3)[C:14]3[CH:22]=[CH:23][CH:24]=[CH:25][C:13]=3[N:12]=2)[CH2:6][CH2:5]1.C1(C2CCC(=O)[O:34][C:33]2=O)C=CC=CC=1>CN(C)C=O>[OH2:18].[O:18]1[CH:19]=[CH:20][CH:21]=[C:17]1[CH2:16][N:15]1[C:14]2[CH:22]=[CH:23][CH:24]=[CH:25][C:13]=2[N:12]=[C:11]1[NH:10][CH:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][NH:1][CH:33]=[O:34])[CH2:5][CH2:6]1.[O:18]1[CH:19]=[CH:20][CH:21]=[C:17]1[CH2:16][N:15]1[C:14]2[CH:22]=[CH:23][CH:24]=[CH:25][C:13]=2[N:12]=[C:11]1[NH:10][CH:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][NH:1][CH:33]=[O:34])[CH2:5][CH2:6]1参加物
4
反応条件
- 温度
- 50 °C
実験手順
A mixture of 5.09 parts of N-[1-(2-aminoethyl)-4-piperidinyl]-1-(2-furanylmethyl)-1H-benzimidazol-2-amine and 54 parts of N,N-dimethylformamide was stirred and heated at 50° C. and there was added dropwise a solution of 2.8 parts of dihydro-3-phenyl-2H-pyran-2,6(3H)dione in 18 parts of N,N-dimethylformamide. Upon completion, stirring was continued overnight at 50° C. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was from a mixture of acetonitrile and 2,2'-oxybispropane, yielding 1.8 parts of N-[2-[4-[[1-(2-furanylmethyl)-1H-benzimidazol-2-yl]amino]-1-piperidinyl]ethyl]formamide hemihydrate; mp. 125.2° C. (compound 46).