HRID1186028

反应详情

EQUATION

反应方程式

HRID 1186028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phenylamine (56 mg) was added to the compound (120 mg) prepared in Example 4 in methanol solution (3 mL) and stirred for 4 hours at room temperature. The reaction mixture was added to sodium borohydride (37 mg) and stirred for 1.5 hours. To alkalinize, 5 mol/L sodium hydroxide solution was added to the concentrated reaction mixture and then extracted with ethyl acetate. The organic layer was washed with saturated sodium and dried by anhydrous sodium sulfate, and then concentrated to obtain the titled compound (124 mg) having the following physical data by purifying the obtained residue by silica gel column chromatography (diethyl ether:hexane=1:2).

WORKUP

后处理

  1. stirringstirred for 1.5 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated sodium
  4. dry with materialdried by anhydrous sodium sulfate
  5. concentrationconcentrated