HRID356643

反应详情

EQUATION

反应方程式

HRID 356643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension mixture of (R)-(-)-2-phenylglycinol(686 mg, 5 mmol), 1,5-dibromopentane (0.82 ml, 6 mmol), and K2CO3 (1.38 g, 10 mmol) in ethanol (15 ml) was refluxed with stirring for 23 h. After cooling down to rt, the white solid was removed by filtration and the filtrate was concentrated to give white solid oil mixture. This was suspended in CH2Cl2 (30 ml), washed with water and saturated NaHCO3 aqueous solution, dried (Na2SO4), and concentrated to give 1.42 g of clear yellow oil. This was purified by column chromatography (silica gel: 50 g, CH2Cl1 /MeOH:30/1 to 20/1) to afford 955 mg (93%) of desired compound as clear light yellow oil.

WORKUP

后处理

  1. temperaturewas refluxed
  2. customthe white solid was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. customto give white solid oil mixture
  5. washwashed with water and saturated NaHCO3 aqueous solution
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated