HRID473022
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
- 50 °C
PROCEDURE
实验过程
To a solution of compound 6 (40 mg, 0.11 mmol) in DCM (3 mL) was added TiCl4 (0.22 mL, 0.22 mmol) and the mixture was stirred in microwave at 50° C. for 10 min. After the reaction, bis-trimehtlysilylcarbodiimide (62 mg, 0.33 mmol) was added and the mixture was stirred in microwave at 60° C. for 10 min. The reaction was quenched with ice water and extracted with CH2Cl2, the organic layer was washed with water, brine, dried and concentrated to give the product 7 (20 mg, 57%).
WORKUP
后处理
- customAfter the reaction, bis-trimehtlysilylcarbodiimide (62 mg, 0.33 mmol)
- additionwas added
- stirringthe mixture was stirred in microwave at 60° C. for 10 min
- customThe reaction was quenched with ice water
- extractionextracted with CH2Cl2
- washthe organic layer was washed with water, brine
- customdried
- concentrationconcentrated