HRID17851

反应详情

EQUATION

反应方程式

HRID 17851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringAfter stirring for 2 hours at ambient temperature
  2. extractionthe mixture is extracted three times with ethyl acetate (30 mL)
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationfiltered
  5. customThe filtrate is evaporated to dryness
  6. dissolutionthe residue is re-dissolved in methanol (5 mL)
  7. additionWater (50 mL) is added to the solution
  8. customthe precipitate obtained
  9. filtrationis collected by filtration
  10. washwashed with water
  11. customdried