反应详情

A suspension of 70.6 g (0.32 mol) of the compound from Example XXXVIII and 3.48 g (0.06 mol) of sodium methylate in 0.5 l of methanol is heated under reflux for 3 hours, the pH is brought to 6.5 with 1N hydrochloric acid at 25° C., the mixture is concentrated in vacuo, the residue is taken up in methylene chloride, the mixture is washed with saturated sodium chloride solution, the organic phase is dried over sodium sulphate and concentrated and the residue is crystallised from diethyl ether/petroleum ether mixtures.

1. temperatureis heated
2. temperatureunder reflux for 3 hours
3. concentrationthe mixture is concentrated in vacuo
4. washthe mixture is washed with saturated sodium chloride solution
5. dry with materialthe organic phase is dried over sodium sulphate
6. concentrationconcentrated
7. customthe residue is crystallised from diethyl ether/petroleum ether mixtures