反应详情

温度

20 °C

A sodium methoxide solution made from 0.40 g (17.391 mmol) of sodium and 65 ml of methanol is added to a solution of 10.30 g (84.355 mmol) of the compound from Example II in 30 ml of methanol, and the mixture is stirred at 20° C. for 72 hours. 5.44 g (101.682 mmol) of ammonium chloride (powdered) and 17.39 mmol (1.04 ml) of acetic acid are added, and the mixture is stirred at 40° C. for 28 hours and cooled. Insoluble salt is filtered off with suction (1.78 g), and the filtrate is concentrated, concentrated with acetone and then stirred with acetone, filtered off with suction and washed.

1. stirringthe mixture is stirred at 40° C. for 28 hours
2. temperaturecooled
3. filtrationInsoluble salt is filtered off with suction (1.78 g)
4. concentrationthe filtrate is concentrated
5. concentrationconcentrated with acetone
6. stirringstirred with acetone
7. filtrationfiltered off with suction
8. washwashed