HRID427295

反应详情

EQUATION

反应方程式

HRID 427295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2-ethyl-4-methoxybenzothiazole-7-carboxylic acid (0.1 g) in dichloromethane (10 ml) was added oxalyl chloride (0.08 ml) and dimethylformanide (1 drop). The reaction was stirred at room temperature for 16 hrs, and then the solvent was removed in vacuo to yield a brown solid residue. This was taken up in dichloromethane is (30 ml) and 3,5-dimethylisoxazol-4-amine (0.05 g) was added followed by triethylamine (0.15 ml) and the reaction stirred at room temperature for 16 hrs. The solvent was removed in vacuo and the product purified by flash chromatography (eluent ethyl acetate) to yield the title compound as an off-white solid (0.016 g). TLC Rf 0.38 (ethyl acetate); Mpt 85-87° C.

WORKUP

后处理

  1. customthe solvent was removed in vacuo
  2. customto yield a brown solid residue
  3. additionwas added
  4. stirringthe reaction stirred at room temperature for 16 hrs
  5. customThe solvent was removed in vacuo
  6. customthe product purified by flash chromatography (eluent ethyl acetate)