HRID17851
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
PROCEDURE
实验过程
N,N′-carbonyldiimidazole (0.6 g) is added to a solution of the compound of Example 78 (3.5 mmol) in DMF (7 mL). After stirring for 1 hour at ambient temperature, phenol (0.5 g) and DBU (0.5 mL) are added. After stirring for 2 hours at ambient temperature, water (40 mL) is added and the mixture is extracted three times with ethyl acetate (30 mL). The organic phases are combined, dried over anhydrous MgSO4 and filtered. The filtrate is evaporated to dryness and the residue is re-dissolved in methanol (5 mL). Water (50 mL) is added to the solution and the precipitate obtained is collected by filtration, washed with water and dried to yield the title product in the form of a white solid.
WORKUP
后处理
- stirringAfter stirring for 2 hours at ambient temperature
- extractionthe mixture is extracted three times with ethyl acetate (30 mL)
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- customThe filtrate is evaporated to dryness
- dissolutionthe residue is re-dissolved in methanol (5 mL)
- additionWater (50 mL) is added to the solution
- customthe precipitate obtained
- filtrationis collected by filtration
- washwashed with water
- customdried