HRID1707772

反应详情

EQUATION

反应方程式

HRID 1707772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a solution of methyl 2-acetyl-5,9-dimethyl-10-(2-tetrahydropyranyl)oxy-4,8-decadienate (370 mg, 1.05 mmol) in methylsulfoxide (2 ml) were added sodium chloride (180 mg, 3.08 mmol) and water (0.1 ml), and the mixture was stirred at 150° C. After four hours, the reaction mixture was allowed to cool to room temperature, and water (15 ml) was added thereto. The product was extracted with ether (20 mlx2). The extract was dried over Na2SO4, and concentrated to give a residue, which was then purified with silica gel column chromatography to obtain 6,10-dimethyl-11-(2-tetrahydropyranyl)oxy-5,9-undecadien-2-one (70%). IR(film)cm-1 ; 2950, 2880, 1720, 1442, 1358, 1120, 1078, 1024, 905, 870, 815.

WORKUP

后处理

  1. temperatureto cool to room temperature
  2. extractionThe product was extracted with ether (20 mlx2)
  3. dry with materialThe extract was dried over Na2SO4
  4. concentrationconcentrated
  5. customto give a residue, which
  6. customwas then purified with silica gel column chromatography