HRID1107347
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
PROCEDURE
实验过程
A stirred mixture of 4,5-diamino-2-(2-propoxyphenyl)pyrimidin-6-one sulphate (1.25 g), glyoxal hydrate (0.4 g), water (62.5 ml) and n-butanol (1 ml) was heated under reflux for one hour to afford a crude product (0.97 g) which was collected and washed with water. The crude product together with another sample (0.12 g) similarly prepared was eluted from a silica column with chloroform. The combined fractions containing product were evaporated under reduced pressure to afford a solid (0.96 g) which was recrystallized from ethanol-water to afford the title compound, 0.8 g, m.p. 177.5-178.5° C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for one hour
- customto afford a crude product (0.97 g) which
- customwas collected
- washwashed with water
- customThe crude product together with another sample (0.12 g) similarly prepared
- washwas eluted from a silica column with chloroform
- additionThe combined fractions containing product
- customwere evaporated under reduced pressure