HRID1696864

反应详情

EQUATION

反应方程式

HRID 1696864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a stirring solution of 3,5-dimethyl-1-H-[1,2,4]-triazole (0.502 g, 5.16 mmol) in THF (36.9 ml) was added NaH (0.199 g, 4.98 mmol). After stirring at RT for 10 mins 2-bromo-3-oxo-butyric acid benzyl ester (step 1) (1.0 g, 3.69 mmol) was added. The mixture was stirred at 40° C. for 30 mins and then allowed to cool to RT. The mixture was absorbed onto silica and purification by chromatography on silica eluting with 0-10% DCM/MeOH afforded the title compound as an orange oil; LC-MS Rt 1.95 mins; MS m/z 288.3 [M+H]+; Method LowpH_v001.

WORKUP

后处理

  1. additionwas added
  2. temperatureto cool to RT
  3. customThe mixture was absorbed onto silica and purification by chromatography on silica eluting with 0-10% DCM/MeOH