反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Sodium dithionite (30 g.) was added in portions to an agitated suspension of 4-amino-2-benzyl-5-phenylazo-pyrimid-6-one (14 g.) in a mixture of ethanol (200 ml.) and 2N aqueous sodium hydroxide solution (200 ml.) maintained at a temperature near to the reflux temperature. The mixture was then heated under reflux for 20 minutes, treated with a further quantity of sodium dithionite (20 g.) and the mixture heated under reflux for a further 30 minutes. The mixture was then evaporated to dryness, the residue was dissolved in water (200 ml.), acidified to pH 6 by means of concentrated hydrochloric acid, cooled to 0° C, and filtered. The solid thus obtained was recrystallised from water to give 4,5-diamino-2-benzyl-pyrimid-6-one (4.4 g.), m.p. 243°-246° C.
WORKUP
后处理
- temperaturemaintained at a temperature near to the reflux temperature
- temperatureThe mixture was then heated
- temperatureunder reflux for 20 minutes
- temperaturethe mixture heated
- temperatureunder reflux for a further 30 minutes
- customThe mixture was then evaporated to dryness
- dissolutionthe residue was dissolved in water (200 ml.)
- filtrationfiltered
- customThe solid thus obtained
- customwas recrystallised from water