HRID1582762

反应详情

EQUATION

反应方程式

HRID 1582762 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.00 g 23.0 mmol of 4-Cyano-5-methyl-4-phenylhexanol disclosed in Example 2 or 3 of JP 11-70613-A was added to and dissolved in acetonitrile 150 ml and triethylamine 3.53 ml. Mesyl chloride, 1.96 ml 25.3 mmol, was added thereto. After 25 minutes, sodium iodide 20.7 g was added thereto. The reaction mixture was partitioned by adding brine and ethyl acetate. The organic layer was washed with aqueous sodium thiosulfate and then with brine, dried over magnesium sulfate, and evaporated. The residue was purified by silica gel column chromatography (ethyl acetate/hexane system), whereby the title compound, 5. 89 g 18.0 mmol, 78.2%, was obtained as a pale yellow oil.

WORKUP

后处理

  1. additionwas added to and
  2. customThe reaction mixture was partitioned
  3. additionby adding brine and ethyl acetate
  4. washThe organic layer was washed with aqueous sodium thiosulfate
  5. dry with materialwith brine, dried over magnesium sulfate
  6. customevaporated
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane system), whereby the title compound, 5
  8. custom89 g 18.0 mmol, 78.2%, was obtained as a pale yellow oil