HRID2410918

反应详情

EQUATION

反应方程式

HRID 2410918 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

To a mixture of 7-amino-3-bromo-9H-carbazole-1-carboxamide 470B (1 g, 2.79 mmol) and CH2I2 (15 mL) was slowly added isopentyl nitrite (1 mL, 7.48 mmol). The mixture was heated in microwave at 60° C. for 45 mins copper(I) iodide (0.266 g, 1.397 mmol) was added to the reaction mixture and heated in microwave at 55° C. for additional 30 mins The mixture was concentrated. EtOAc(50 ml) was added and stirred for 10 mins and filtered. The collected solid was washed with H2O 2×50 ml. The remaining solid was purified using preparative HPLC to give titled product. MS (ESI) m/z 412.82 (M−H)−.

WORKUP

后处理

  1. additionwas added to the reaction mixture
  2. concentrationwas concentrated
  3. additionEtOAc(50 ml) was added
  4. filtrationfiltered
  5. washThe collected solid was washed with H2O 2×50 ml
  6. customThe remaining solid was purified