HRID733165
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A suspension of 2-methylsulfanyl-6-propyl-pyrimidin-4-ol (15.5 g) in phosphorous oxychloride (160 mL) was refluxed for 6 hours. The solvent was distilled off under reduced pressure. The residue was diluted with dichloromethane and poured in ice. The layers were separated, then the aqueous layer was extracted twice with ethyl acetate. The combined organic layers were dried over sodium sulphate, filtered and concentrated under reduced pressure to afford 4-chloro-2-methylsulfanyl-6-propyl-pyrimidine (17.5 g, 100%) as an orange oil.
WORKUP
后处理
- temperaturewas refluxed for 6 hours
- distillationThe solvent was distilled off under reduced pressure
- additionThe residue was diluted with dichloromethane
- additionpoured in ice
- customThe layers were separated
- extractionthe aqueous layer was extracted twice with ethyl acetate
- dry with materialThe combined organic layers were dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure