HRID2244402

反应详情

EQUATION

反应方程式

HRID 2244402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-methyl-pyridin-4-ylamine (0.10 g, 0.91 mmol) in dry dioxane (2.00 ml) was added to a 2N solution of trimethylaluminium in heptane (0.46 ml, 0.91 mmol). The mixture was stirred at room temperature for 1 h, then 2-methyl-5-(pyridin-3-ylamino)-thiazole-4-carboxylic acid ethyl ester (0.08 g, 0.30 mmol) was added and the reaction mixture was irradiated in a microwave oven at 150° C. for 15 min. The mixture was quenched with water (1.00 ml) and diluted with dichloromethane. After drying with sodium sulphate, the solvent was evaporated. The residue was purified by flash chromatography (dichloromethane/methanol) yielding the title compound (0.04 g, 41%) as a yellow solid, MS (ISP): m/e=326.1 (M+H+).

WORKUP

后处理

  1. customthe reaction mixture was irradiated in a microwave oven at 150° C. for 15 min
  2. customThe mixture was quenched with water (1.00 ml)
  3. additiondiluted with dichloromethane
  4. dry with materialAfter drying with sodium sulphate
  5. customthe solvent was evaporated
  6. customThe residue was purified by flash chromatography (dichloromethane/methanol)