HRID1703075

反应详情

EQUATION

反应方程式

HRID 1703075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 750 ml. of dichloromethane, 37.2 g. of 11-phenyl-1-undecanol (prepared as described in Example 6) and 32 ml. of triethylamine cooled in an ice-salt bath to -10° C. is added dropwise, over 15 minutes, 13.2 ml. of methanesulfonyl chloride. The mixture is cooled at -10° C. to -15° C. for 30 minutes and then washed with 300 ml. of cold water, 300 ml. of cold 10% hydrochloric acid, 300 ml. of cold 5% sodium carbonate and with 200 ml. of cold, saturated, sodium chloride solution. The organic layer is dried over magnesium sulfate and concentrated in vacuo to give a pale yellow oil.

WORKUP

后处理

  1. additionTo a mixture of 750 ml
  2. additionis added dropwise, over 15 minutes
  3. temperatureThe mixture is cooled at -10° C. to -15° C. for 30 minutes
  4. washwashed with 300 ml
  5. dry with materialThe organic layer is dried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customto give a pale yellow oil