反应详情

温度

20 °C

10.30 g (84.355 mmol) of the compound from Example II are dissolved in 30 ml of methanol. The solution is admixed with a solution of 0.40 g (17.391 mmol) of sodium in 65 ml of methanol and stirred at 20° C. for 72 hours. 5.44 g (101.682 mmol) of ammonium chloride (ground in a mortar) 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 subsequently 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. stirringsubsequently stirred with acetone
7. filtrationfiltered off with suction
8. washwashed