HRID81889

反应详情

EQUATION

反应方程式

HRID 81889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,2-Diamino-2-methylpropane (8.4 mL, 80.0 mmol) was added to a chilled (0° C.) solution of 4-chloro-3-nitro[1,5]naphthyridine (15.2 g, 72.7 mmol) and triethylamine (20.2 mL, 145 mmol) in dichloromethane (350 mL). The reaction mixture was stirred overnight and then concentrated under reduced pressure. The residue was combined with water (300 mL) and heated at reflux with stirring for 1 hour. The reaction mixture was cooled and filtered. The isolated solid was washed with water and then dried under high vacuum to provide 18.5 g of N1-(3-nitro[1,5]naphthyridin-4-yl)-2-methylpropane-1,2-diamine as a bright yellow powder.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. temperatureheated
  3. temperatureat reflux
  4. stirringwith stirring for 1 hour
  5. temperatureThe reaction mixture was cooled
  6. filtrationfiltered
  7. washThe isolated solid was washed with water
  8. customdried under high vacuum