反应详情

温度

50 °C

To a solution of N,N′-di-tert-butoxycarbonyl-7-(piperidin-4-ylmethoxy)-1,2,3,4-tetrahydroisoquinoline-2-carboxamidine (100 mg) in a mixture of tetrahydrofuran (1 ml) and dimethylformamide (1 ml) were added 9.1N sodium hydroxide (0.068 ml) and 4-picolyl chloride hydrochloride (51 mg), and the mixture was stirred at 50° C. for 5 hours. After completion of the reaction, water was added and the mixture was extracted with ethyl acetate and was washed successively with water and saturated brine. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated. The obtained residue was purified by preparative thin layer chromatography (chloroform:methanol=20:1) and dried under reduced pressure to give the title compound (93 mg).

1. additionwas added
2. extractionthe mixture was extracted with ethyl acetate
3. washwas washed successively with water and saturated brine
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. customthe solvent was evaporated
6. customThe obtained residue was purified by preparative thin layer chromatography (chloroform:methanol=20:1)
7. customdried under reduced pressure