反应详情

温度

5 °C

0.48 ml of acetic anhydride dissolved in 5 ml of methylene chloride is added to a solution of 2 g (0.005 mole) of N-[1-[1-[(4-fluorophenyl)methyl]-2-(1H)-benzimidazolyl]-4-piperidinyl]-N,N'-dimethylguanidine in 20 ml of methylene chloride, cooled to 5° C. Stirring is continued for 2 h and the mixture is then poured into concentrated sodium hydroxide. The phases are separated, the organic phase is dried with MgSO4, is filtered and is evaporated down. On addition of acetone, the product crystallizes. It is purified by chromatography on a silica column (eluent 9/1 methylene chloride/methanol) N-[1-[1-[(4-fluorophenyl)methyl]-2(1H)-benzimidazolyl]-4-piperidinyl]-N,N'-dimethyl-N"-acetylguanidine is obtained.

1. customThe phases are separated
2. dry with materialthe organic phase is dried with MgSO4
3. filtrationis filtered
4. customis evaporated down
5. additionOn addition of acetone
6. customthe product crystallizes
7. customIt is purified by chromatography on a silica column (eluent 9/1 methylene chloride/methanol) N-[1-[1-[(4-fluorophenyl)methyl]-2(1H)-benzimidazolyl]-4-piperidinyl]-N,N'-dimethyl-N"-acetylguanidine
8. customis obtained