HRID871863

反应详情

EQUATION

反应方程式

HRID 871863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 0.60 g (1.51 mmol) of the product prepared in step 11.3 and 0.53 g (3.02 mmol) of 4-morpholin-4-ylphenylamine in 6.5 mL of NMP is placed in a 10 mL microwave tube. The sealed tube is placed in the microwave oven (CEM machine, Discovery model) and the mixture is heated under pressure at 120°C. for 60 minutes at a power of 75 W, and then cooled to room temperature. 15 mL of water and then 5 mL of saturated aqueous NaHCO3 are added and the precipitate formed is drained by suction and then dried in an oven. The crude solid is triturated in methanol, drained by suction and dried in an oven under vacuum. 0.159 g of the expected product is obtained in solid form. Yield=20%.

WORKUP

后处理

  1. customis placed in a 10 mL microwave tube
  2. temperaturecooled to room temperature
  3. customthe precipitate formed
  4. customdried in an oven
  5. customThe crude solid is triturated in methanol
  6. customdried in an oven under vacuum