HRID1848561
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
- 0 °C
PROCEDURE
实验过程
To a solution of the product of Step J (340 mg, 0.723 mmol) in methylene chloride (30 mL) was added PCC (311 mg, 1.45 mmol) at 0° C. and the resulting solution was stirred at 0° C. for 2 h. The reaction mixture was partitioned between methylene chloride and saturated bicarbonate, and the alkaline phase was extracted with methylene chloride (3×50 mL). The combined organic phase was dried over sodium sulfate, concentrated and the residue was purified on TLC using 10% methanol/methylene chloride as developing solvents to give the title compound. LC/MS: (M+1)+: 469.20.
WORKUP
后处理
- customThe reaction mixture was partitioned between methylene chloride and saturated bicarbonate
- extractionthe alkaline phase was extracted with methylene chloride (3×50 mL)
- dry with materialThe combined organic phase was dried over sodium sulfate
- concentrationconcentrated
- customthe residue was purified on TLC