HRID1457186
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
A mixture of the title compound of Step (C), 1H-1,2,3-triazole (144 mg, 2.1 mmol) and K2CO3 (1.3 g, 9.5 mmol) in 3.8 ml sulfolane was heated at 140° C. for 3 hrs. After cooling, 30 ml H2O was added and the mixture was extracted with 1:1 EtOAc/hexane. The combined organic extracts were washed with H2O and brine, dried and concentrated. The residue was chromatographed on silica gel using 3:1 hexane/EtOAc to afford the title compound of this step (256 mg, 44% for three steps).
WORKUP
后处理
- temperatureAfter cooling
- extractionthe mixture was extracted with 1:1 EtOAc/hexane
- washThe combined organic extracts were washed with H2O and brine
- customdried
- concentrationconcentrated
- customThe residue was chromatographed on silica gel using 3:1 hexane/EtOAc