HRID1019536

反应详情

EQUATION

反应方程式

HRID 1019536 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

Add, dropwise, 4.7 g (80.76 mmol) of azetidine to a suspension, stirred at 20° C., of 27.9 g (0.201 mole) of potassium carbonate and 11 g (67.3 mmol) of 2-chloro-5-nitropyridine in 100 mL of dimethylformamide. Stir the mixture for 5 minutes at 20° C., then for 6 hours at 70° C. After this time, the suspension is poured into a mixture of 300 mL of water and 300 mL of ethyl acetate. The aqueous phase is separated, then extracted with 200 mL of ethyl acetate. The organic phases are combined, washed three times with 250 mL of water, then dried over sodium sulfate and concentrated at reduced pressure. We thus obtain 11.7 g of the expected product in the form of a solid.

WORKUP

后处理

  1. additionAdd
  2. waitfor 6 hours at 70° C
  3. customThe aqueous phase is separated
  4. extractionextracted with 200 mL of ethyl acetate
  5. washwashed three times with 250 mL of water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated at reduced pressure