HRID2204321

反应详情

EQUATION

反应方程式

HRID 2204321 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of methanesulfonic acid 1,3-dimethyl-2-oxo-hexahydro-pyrimidin-5-yl ester (Step P6) (3.2 g, 14.3 mmol) in DMF (75 mL) at rt was added sodium azide (1.9 g, 28.7 mmol) and the mixture was stirred at 70° C. for 13 h. The mixture was diluted with CH2Cl2/isopropanol 3:1 and extracted with a saturated aqueous NaHCO3 solution. The organic phase was dried (Na2SO4), filtered and concentrated to afford the title compound. ESI-MS: [M+H]+ 170.1 (MS 1).

WORKUP

后处理

  1. extractionextracted with a saturated aqueous NaHCO3 solution
  2. dry with materialThe organic phase was dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated