HRID1715687

反应详情

EQUATION

反应方程式

HRID 1715687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
87.5 °C

PROCEDURE

实验过程

A mixture of 4-[(4-fluorophenyl)sulfonyl]morpholine (0.25 g, 1 mmol), cesium carbonate (1.30 g, 4 mmol), and guanidine carbonate (1.08 g, 6 mmol) in 2 ml of 1-methyl-2-pyrrolidinone (NMP) is stirred at 85 to 90° C. for 24 hrs. It is then cooled to room temperature and diluted with ether. The resulting suspension is filtered, and the precipitate extracted with tetrahydrofuran (THF) to yield, after evaporation of solvent, 0.12 g of a yellow solid; mp 102-105° C.; MS (ESI) m/z 285.1 (M+H); HRMS: calcd for C11H16N4O3S, 284.0943; found (ESI_FT), 285.1011 (M+H).

WORKUP

后处理

  1. temperatureIt is then cooled to room temperature
  2. filtrationThe resulting suspension is filtered
  3. extractionthe precipitate extracted with tetrahydrofuran (THF)
  4. customto yield
  5. customafter evaporation of solvent, 0.12 g of a yellow solid