HRID6815
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 mixture of the product of Step E, (66 mg) in anhydrous diglyme (2 mL) was added 4-trifluoromethylphenylpropionic acid (1.1 eq.) and EDC (2 eq.). The reaction mixture was heated to 50° C. overnight. After approximately 18 h, the mixture was heated at 110° C. for 2 hr. The mixture was cooled to r.t., quenched with water and extracted with excess EtOAc. The combined extracts were dried over a drying agent filtered and the solvent removed under vacuum. The residue was purified by preparative TLC eluting with EtOAc to afford the product, MS: m/z 538.
WORKUP
后处理
- temperaturethe mixture was heated at 110° C. for 2 hr
- temperatureThe mixture was cooled to r.t.
- customquenched with water
- extractionextracted with excess EtOAc
- customThe combined extracts were dried over a drying agent
- filtrationfiltered
- customthe solvent removed under vacuum
- customThe residue was purified by preparative TLC
- washeluting with EtOAc
- customto afford the product, MS