HRID2284894

反应详情

EQUATION

反应方程式

HRID 2284894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2,4,5-trichloropyrimidine (5 g, 27.32 mmol) in THF:water (1:1, 40 mL), was added sodium thiomethoxide (2.15 g, 30.01 mmol) at 0° C., and the mixture was stirred at rt for 4 h. TLC showed completion of starting material and formation of a slightly polar spot (TLC system: hexane charred in iodine). The reaction mixture was concentrated, water (20 ml) was added, and the product was extracted with ethyl acetate (2×20 ml). The organic layer was dried over sodium sulfate and concentrated to afford the desired compound as a white solid (5 g, 94.8%). MS m/z: 195.2 (ES+, M+H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionwater (20 ml) was added
  3. extractionthe product was extracted with ethyl acetate (2×20 ml)
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. concentrationconcentrated