HRID635156

反应详情

EQUATION

反应方程式

HRID 635156 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

To a cooled (0° C.), stirred solution of 2-methyl-3-cyclohexylpropanol (40.3 g., 0.26 mol.), dimethylaminopyridine (2.5 g., 0.02 mol.), and triethylamine (38.4 g., 0.38 mol.) in 200 ml of toluene was added acetic anhydride (39.4 g. 0.39 mol) over 30 minutes. The resulting solution was allowed to warm to room temperature and stirred for an additional 1.5 hours. The reaction mixture was washed twice with 125 ml portions of 2 N aqueous sodium chloride, dried over magnesium sulfate and concentrated to a colorless oil which was distilled to obtain 72 g. 98% yield; bp 67-71° C. at 0.6 mm. Odor: very pleasant fruity, rosy, floral. Mass Spectrum from 5508-36. MS (El) m/z (relative intensity) 155 (M+−C2H3O, 2), 138 (M+−C2H4O2, 15).

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. washThe reaction mixture was washed twice with 125 ml portions of 2 N aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated to a colorless oil which
  5. distillationwas distilled
  6. customto obtain 72 g