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
Ethyl 7-oxo-5,6,7,8-tetrahydroimidazo[1,2-a]pyrimidine-2-carboxylate (1.711 mmol, 0.358 g) was dissolved in ethanol (5 ml) and cooled to 0° C. 1N solution of NaOH (5 ml) was slowly added. The resulting mixture was heated to 60° C. for 1.5 h. Ethanol was evaporated, the residue diluted with tert-butyl methyl ether and acidified with 2 N HCl solution under cold conditions. The mixture was stirred for overnight. DCM and water was added and the precipitate was filtered. Phases in the filtrate were separated and the water phase was evaporated. The residue from water and precipitate were combined. 0.592 g of the title compound was obtained. 1H-NMR (400 MHz, DMSO-d6): δ 2.73 (t, 2H), 4.12 (t, 2H), 7.58 (s, 1H), 11.09 (bs, 1H).
WORKUP
后处理
- temperatureThe resulting mixture was heated to 60° C. for 1.5 h
- customEthanol was evaporated
- additionthe residue diluted with tert-butyl methyl ether
- additionDCM and water was added
- filtrationthe precipitate was filtered
- customPhases in the filtrate were separated
- customthe water phase was evaporated