HRID1668912

反应详情

EQUATION

反应方程式

HRID 1668912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

1-Chloro-6-methyl-5-nitroisoquinoline (0.25 g, 1.1 mmol) and 3-(trifluoromethyl)benzenamine (0.17 mL, 1.3 mmol) were added to a microwave tube containing 3 mL of isopropanol. The tube was capped and heated at 180° C. for 1500 seconds. The volatiles were removed in vacuo. The residue was taken up in DCM and washed with saturated NaHCO3. The organic layer was dried with sodium sulfate and purified by column chromatography on silica gel using a gradient of 10 to 40% of ethyl acetate in hexanes to give the product as an orange solid (0.31 g, 79%). MS (M+H)+ 348.

WORKUP

后处理

  1. customThe tube was capped
  2. customThe volatiles were removed in vacuo
  3. washwashed with saturated NaHCO3
  4. dry with materialThe organic layer was dried with sodium sulfate
  5. custompurified by column chromatography on silica gel using a gradient of 10 to 40% of ethyl acetate in hexanes