HRID1435837

反应详情

EQUATION

反应方程式

HRID 1435837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (5-methyl-3-phenyl-4-isoxazolyl)methylamine (2.4 g, 12.7 mmol) and 5-chloro-pyrazine-2-carboxylic acid methyl ester (2.2 g, 12.7 mmol) in DMSO (15 mL) was heated with microwave irradiation to 160° C. for 30 min. After cooling to room temperature the reaction mixture was extracted (ethyl acetate/water). The organic phase was dried over sodium sulfate, concentrated and chromatographed (SiO2, heptane:ethyl acetate=100:0 to 20:80). The oily product obtained was triturated with diisopropylether and ethyl acetate to afford the title compound (3.5 g, 84% as an off-white solid. MS: m/e=325.4 [M+H]+.

WORKUP

后处理

  1. extractionwas extracted (ethyl acetate/water)
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. concentrationconcentrated
  4. customchromatographed (SiO2, heptane:ethyl acetate=100:0 to 20:80)
  5. customThe oily product obtained
  6. customwas triturated with diisopropylether and ethyl acetate