HRID1168731

反应详情

EQUATION

反应方程式

HRID 1168731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of norharmane (2.0 g, 11.9 mmol) in water (89 ml) and 1M aqueous HCl (29.8 ml, 29.8 mmol) was added N-chlorosuccinimide (3.17 g, 23.8 mmol) portionwise. The resulting solution was stirred at RT for 6 h, and then at 0° C. to 5° C. for 12 h. The reaction was diluted with water (100 ml) and basified cautiously with solid K2CO3 (4.3 g). After stirring at RT for 1 h, the product was collected and washed with water. The crude product was refluxed in chloroform for 1 h and filtered after cooling to 15° C. to provide 2.05 g of 7-chloro-β-carboline.

WORKUP

后处理

  1. waitat 0° C. to 5° C. for 12 h
  2. stirringAfter stirring at RT for 1 h
  3. customthe product was collected
  4. washwashed with water
  5. temperatureThe crude product was refluxed in chloroform for 1 h
  6. filtrationfiltered
  7. temperatureafter cooling to 15° C.