HRID1191306

反应详情

EQUATION

反应方程式

HRID 1191306 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a solution of 4-(3-cyanophenyl)-1H-benzo[h]quinazolin-2-one (112 mg, 0.377 mmol) in DMF (2 mL) was added tri-n-butyltin azide (312 μL, 1.13 mmol), and stirred at 110° C. for 18 hours. After cooled to room temperature, the reaction mixture was poured into 1M sodium hydroxide, and washed with ethyl acetate. After aqueous layer was neutralized with 1M hydrochloric acid, the precipitated solid was collected by filtration, washed with methanol, and with water. The obtained crystal was dried to give the titled compound as a yellow crystal (70 mg, yield 55%).

WORKUP

后处理

  1. temperatureAfter cooled to room temperature
  2. washwashed with ethyl acetate
  3. filtrationthe precipitated solid was collected by filtration
  4. washwashed with methanol
  5. customThe obtained crystal was dried