反应详情

温度

20 °C

The solution of the product from step (vi) (2.00 g, 5.28 mmol) and methanesulfonic acid (1.52 g, 15.8 mmol) in acetonitrile (16.0 g) was cooled to 20° C. and thionyl chloride (0.94 g, 7.92 mmol) was slowly added to the solution. After the mixture was stirred at 20° C. for 30 minutes, 4-dimethylamino-1-butanol (1.11 g, 9.50 mmol) was slowly added to the mixture. The mixture was heated to 40° C. and stirred at the temperature for 5 hours. After the reaction mixture was cooled to 20° C., ethyl acetate (18.0 g) and 25% aq. trimethylamine (18.0 g) was slowly added to the mixture. The organic layer was separated and washed respectively with 5% aq. NH4Cl (20.0 g), 1% aq. NaCl (20.0 g) and water (20.0 g). The solution of the subtitle compound was used in the next step without concentration.

1. temperatureThe mixture was heated to 40° C.
2. stirringstirred at the temperature for 5 hours
3. temperatureAfter the reaction mixture was cooled to 20° C.
4. customThe organic layer was separated
5. washwashed respectively with 5% aq. NH4Cl (20.0 g), 1% aq. NaCl (20.0 g) and water (20.0 g)
6. concentrationThe solution of the subtitle compound was used in the next step without concentration