HRID1059351

反应详情

EQUATION

反应方程式

HRID 1059351 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

386 mg of 3-(tert-butoxycarbonyl)-3-azabicyclo[3.3.0]-octan-7-one synthesized in accordance with the method described in Tetrahedron, 49, 5047 (1993) was dissolved in 20 ml of ethanol. After adding 65 mg of sodium borohydride, the resulting mixture was stirred at room temperature for 30 minutes. Then the reaction mixture was concentrated under reduced pressure, diluted with ethyl acetate, washed with water and a saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate. After filtering, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (eluted with n-hexane/ethyl acetate) to thereby give 319 mg of the title compound as white crystals.

WORKUP

后处理

  1. concentrationThen the reaction mixture was concentrated under reduced pressure
  2. additiondiluted with ethyl acetate
  3. washwashed with water
  4. dry with materiala saturated aqueous solution of sodium chloride and then dried over anhydrous magnesium sulfate
  5. filtrationAfter filtering
  6. distillationthe solvent was distilled off under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (eluted with n-hexane/ethyl acetate)