HRID406198
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of rac-5-(7-ethoxy-7-oxoheptyl)-2,3-diphenyl-5,6,7,8-tetrahydropyrido[2,3-b]pyrazine-7,8-diyl diacetate (step 1) (30 mg, 0.054 mmol) in THF (3 ml) and water (1.0 ml) was added LiOH (7.70 mg, 0.322 mmol). The suspension was heated to reflux for 1 hour and allowed to stand at RT overnight. The mixture was again heated at reflux for 30 minutes and after cooling to RT, 1M HCl was added to adjust the pH to below pH 5. The volatile solvent was evaporated and the resulting mixture was extracted with EtOAc (10 ml). The organic extract was washed with water, dried over MgSO4, filtered and concentrated in vacuo to afford a mixture of the title products;
WORKUP
后处理
- temperatureThe suspension was heated
- temperatureto reflux for 1 hour
- temperatureThe mixture was again heated
- temperatureat reflux for 30 minutes
- customThe volatile solvent was evaporated
- extractionthe resulting mixture was extracted with EtOAc (10 ml)
- extractionThe organic extract
- washwas washed with water
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto afford