反应详情

A mixture of 3.75 parts of 3-amino-1-propanol, 20.5 parts of 1-(4-fluorophenylmethyl)-N-[1-(2-isothiocyanatoethyl)-4-piperidinyl]-1H-benzimidazol-2-amine and 450 parts of tetrahydrofuran was stirred for 3 hours at room temperature. The reaction mixture was evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (96:4 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile, yielding 16 parts (64%) of N-[2-[4-[[1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-yl]amino]-1-piperidinyl]ethyl]-N'(3-hydroxypropyl)thiourea monohydrate; mp. 124.6° C. (compound 30).

1. customThe reaction mixture was evaporated
2. customThe residue was purified by column chromatography over silica gel using
3. additiona mixture of trichloromethane and methanol (96:4 by volume) as eluent
4. customThe pure fractions were collected
5. customthe eluent was evaporated
6. customThe residue was crystallized from acetonitrile