HRID2184300

反应详情

EQUATION

反应方程式

HRID 2184300 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a suspension of 5,6-diamino-nicotinic acid isopropyl ester (1 eq., 5.1 g) in cyclohexanone (50 ml) bromobutanone (1.2 equiv., 3.4 ml) was added over 10 min. The dark brown mixture was heated to 100° C. (inner temperature) and stirred 1.5 h at this temperature. The suspension was cooled to room temperature and the pale yellow solid was filtered off and was washed with TBME (3×10 ml). Drying under reduced pressure at 45° C. Yield: 6.0 g (74%).

WORKUP

后处理

  1. additionwas added over 10 min
  2. temperatureThe suspension was cooled to room temperature
  3. filtrationthe pale yellow solid was filtered off
  4. washwas washed with TBME (3×10 ml)
  5. customDrying under reduced pressure at 45° C