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
5-methyl-2-thiouracil (2 g, 98%, 13.78 mmol, 1 eq) and KOH, 85%, (1.05 eq, 995 mg) were suspended in 25 ml of absolute ethanol and the mixture was stirred for 1 hour at room temperature. In the suspension was then added MeI (1.05 eq, 905 μl) dropwise and the suspension was heated at 65° C. (temperature on display of heating device) for 2 hours. Solvent was then evaporated. In the rest was added 100 ml of water and using ultrasound was suspended. The obtained precipitate was collected by filtration, it was dried and obtained was 5-methyl-2-methylsulfanyl-1H-pyrimidin-4-one (1.7 g, yield=71.9%, purity=93%) in form of a white powder. MS: [M+H]+=157.08 1H NMR (300 MHz; DMSO-d6) δ/ppm 1.90 (s, 3H), 2.50 (s, 3H), 7.78 (s, 1H)
WORKUP
后处理
- temperature(temperature on display of heating device) for 2 hours
- customSolvent was then evaporated
- additionIn the rest was added 100 ml of water
- filtrationThe obtained precipitate was collected by filtration, it
- customwas dried
- customobtained