HRID2264161

反应详情

EQUATION

反应方程式

HRID 2264161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customquenched with 10 mL of acetic acid
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was partitioned between 100 mL of saturated sodium bicarbonate and 200 mL of ethyl acetate
  4. dry with materialthe extracts dried over MgSO4
  5. concentrationConcentration under reduced pressure
  6. customgave a white crystalline solid