HRID2264158
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 1 g of methyl 2-chloro-6-methylpyrimidine-4-carboxylate, 20 mL of methanol and 2 mL of 30% sodium methoxide in methanol was stirred under nitrogen at room temperature for 3 hrs, quenched with 3 mL of acetic acid and concentrated under reduced pressure. The residue was partitioned between 25 mL of saturated sodium bicarbonate and 3×20 mL of ethyl acetate and the extracts dried over MgSO4. Concentration under reduced pressure gave a white crystalline solid: MS (m+1)=183.1; 1H NMR (400 MHz, CDCl3) 7.5 (s, 1H), 4.1 (s, 3H), 4.0 (s, 3H), 2.58 (s, 3H).
WORKUP
后处理
- customquenched with 3 mL of acetic acid
- concentrationconcentrated under reduced pressure
- customThe residue was partitioned between 25 mL of saturated sodium bicarbonate and 3×20 mL of ethyl acetate
- dry with materialthe extracts dried over MgSO4
- concentrationConcentration under reduced pressure
- customgave a white crystalline solid