HRID2264161
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 mixture of 5 g of ethyl 4-chloro-2-(methylthio)pyrimidine-5-carboxylate, 250 mL of methanol and 5 mL of 30% sodium methoxide in methanol was stirred under nitrogen at room temperature for 5 hrs, quenched with 10 mL of acetic acid and concentrated under reduced pressure. The residue was partitioned between 100 mL of saturated sodium bicarbonate and 200 mL of ethyl acetate and the extracts dried over MgSO4. Concentration under reduced pressure gave a white crystalline solid: MS (m+1)=215.1; 1H NMR (400 MHz, CDCl3) 8.85 (s, 1H), 4.1 (s, 3H), 4.05 (s, 3H), 3.85 (s, 3H).
WORKUP
后处理
- customquenched with 10 mL of acetic acid
- concentrationconcentrated under reduced pressure
- customThe residue was partitioned between 100 mL of saturated sodium bicarbonate and 200 mL of ethyl acetate
- dry with materialthe extracts dried over MgSO4
- concentrationConcentration under reduced pressure
- customgave a white crystalline solid