反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
A mixture of 2.8 parts of 2-(methylthio)thiazolo[5,4-b]pyridine and 5.5 parts of N-[1-(2-aminoethyl)-4-piperidinyl]-1-[(4-fluorophenyl)methyl]-1H-benzimidazol-2-amine was stirred for 24 hours at 140° C. The reaction mixture was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (97:3 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 1.9 parts (25%) of N-[2-[4-[[1-[(4-fluorophenyl)-methyl]-1H-benzimidazol-2-yl]amino]-1-piperidinyl]ethyl]thiazolo-[5,4-b]pyridin-2-amine; mp. 203.5° C. (compound 103).
WORKUP
后处理
- customThe reaction mixture was purified by column chromatography over silica gel using
- additiona mixture of trichloromethane and methanol
- customThe pure fractions were collected
- customthe eluent was evaporated
- customThe residue was crystallized from acetonitrile
- filtrationThe product was filtered off
- customdried