HRID1019575

反应详情

EQUATION

反应方程式

HRID 1019575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 0.311 g (2.84 mmol) of 3-hydroxyazetidine hydrochloride, 0.3 g (1.89 mmol) of 2-chloro-5-nitropyridine and 0.41 mL (2.84 mmol) of triethylamine in 10 mL of dimethylformamide is heated overnight at 100° C. After this time, the suspension is poured into a mixture of 30 mL of water and 30 mL of ethyl acetate. The aqueous phase is separated, and then extracted with 20 mL of ethyl acetate. The organic phases are combined, washed three times with 25 mL of water, then dried over sodium sulfate and concentrated at reduced pressure. We thus obtain 0.34 g of the expected product in the form of a solid, which will be used as it is in the rest of the synthesis.

WORKUP

后处理

  1. customThe aqueous phase is separated
  2. extractionextracted with 20 mL of ethyl acetate
  3. washwashed three times with 25 mL of water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated at reduced pressure
  6. customis in the rest of the synthesis