HRID450179
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
To a solution of sodium methoxide (0.090 g of sodium) in MeOH (12 mL) was added 0.486 g (3.03 mmol) of 2-chloro-5-nitropyrimidine, and the mixture was heated under reflux for 1 hr. After cooling, the mixture was concentrated in vacuo, extracted with EtOAc, and washed with water. The aqueous layer was extracted with CHCl3 and the combined organic layers were dried (Na2SO4), and concentrated, to give 0.347 g (75% yield) of 2-methoxy-5-nitropyrimidine as a yellow powder: 1H NMR (CDCl3) δ9.31 (s, 2H), 4.17 (s, 3H); LCMS (APCI+) m/z: 156 (MH+, 100%).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 1 hr
- temperatureAfter cooling
- concentrationthe mixture was concentrated in vacuo
- extractionextracted with EtOAc
- washwashed with water
- extractionThe aqueous layer was extracted with CHCl3
- dry with materialthe combined organic layers were dried (Na2SO4)
- concentrationconcentrated