HRID1855675

反应详情

EQUATION

反应方程式

HRID 1855675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under the argon atmosphere, dimethyl-(3-phenoxy-2-oxopropyl)-phosphonate (826 mg, 3.20 mmol) and potassium phosphate (679 mg, 3.20 mmol) were added to a THF solution (16 mL) of the compound (634 mg, 1.60 mmol) produced in Example 13, and the mixture was stirred at room temperature for one day. The reaction solution was added to an aqueous saturated ammonium chloride solution, and the aqueous layer was extracted with ethyl acetate two times. The collected organic layers were washed with a saturated saline, and dried with anhydrous sodium sulfate. The solution was concentrated under reduced pressure, and purified with a column apparatus (Hiflash-SI, Size L, hexane→ethyl acetate:hexane=4:6) manufactured by Yamazen Corporation to obtain a titled compound (426 mg) having the following physical property values.

WORKUP

后处理

  1. extractionthe aqueous layer was extracted with ethyl acetate two times
  2. washThe collected organic layers were washed with a saturated saline
  3. dry with materialdried with anhydrous sodium sulfate
  4. concentrationThe solution was concentrated under reduced pressure
  5. custompurified with a column apparatus (Hiflash-SI, Size L, hexane→ethyl acetate:hexane=4:6)