HRID1515108

反应详情

EQUATION

反应方程式

HRID 1515108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Ethylindan-1-one (160 mg, 0.998 mmol) synthesized in (44A) was dissolved in tetrahydrofuran (5 mL), and the resulting solution was cooled to 0° C. Thereafter, sodium borohydride (57 mg, 1.50 mmol) was added thereto, and methanol (2 mL) was added dropwise thereto, and then, the resulting mixture was stirred at room temperature for 8 hours. Water was added to the reaction solution, and the organic matter was extracted with ethyl acetate. The organic layer was washed with water and a saturated sodium chloride solution, then dried over anhydrous magnesium sulfate and filtered. Then, the solvent was distilled off under reduced pressure, whereby a crude product was obtained. This crude product was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 70:30 (v/v)), whereby the objective title compound was obtained as a yellow oily substance (162 mg, yield: 100%).

WORKUP

后处理

  1. extractionthe organic matter was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materiala saturated sodium chloride solution, then dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. distillationThen, the solvent was distilled off under reduced pressure, whereby a crude product
  6. customwas obtained
  7. customThis crude product was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 70:30 (v/v)), whereby the objective title compound
  8. customwas obtained as a yellow oily substance (162 mg, yield: 100%)