HRID907266

反应详情

EQUATION

反应方程式

HRID 907266 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the product of Example 11 (460 mg) in DMF (10 mL) was added 60% sodium hydride (38 mg) and the reaction stirred at room temperature for 30 minutes before the addition of 4-(chloromethyl)phenyl acetate (280 mg). The reaction mixture was then stirred at room temperature for 17 hrs. Additional 60% sodium hydride (38 mg) was added and the reaction was stirred for a further 2 hours. NaOH (5N, 2 mL) was added and the reaction was stirred at room temperature for 90 minutes. The reaction mixture was acidified with HCl (2N) and extracted into ethyl acetate. The organics were washed with water and brine, dried over magnesium sulphate and evaporated to yield the sub-titled compound (500 mg).

WORKUP

后处理

  1. stirringthe reaction was stirred for a further 2 hours
  2. stirringthe reaction was stirred at room temperature for 90 minutes
  3. extractionextracted into ethyl acetate
  4. washThe organics were washed with water and brine
  5. dry with materialdried over magnesium sulphate
  6. customevaporated