HRID1153699

反应详情

EQUATION

反应方程式

HRID 1153699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Approximately 397 g of 50% aqueous sodium hydroxide solution was added dropwise over a period of 7 hours to a solution of n-dodecyl mercaptan (1000g) and 1-chloropropane-2,3-diol (547g) in isopropanol solvent (2000 cc) at ambient temperature. The reaction temperature rose from 21° to 56° C. during the addition. The reaction was refluxed for 5 hours at 80° C. and then filtered hot through paper to remove the precipitated salt. The isopropanol solvent was removed by distillation. The product residue was dissolved in about 4000 cc of toluene and washed with water several times. The toluene solution was dried over magnesium sulfate and filtered through diatomaceous earth. Toluene was removed by high speed rotary evaporation to yield a white solid product.

WORKUP

后处理

  1. additionThe reaction temperature rose from 21° to 56° C. during the addition
  2. filtrationfiltered hot through paper
  3. customto remove the precipitated salt
  4. customThe isopropanol solvent was removed by distillation
  5. dissolutionThe product residue was dissolved in about 4000 cc of toluene
  6. washwashed with water several times
  7. dry with materialThe toluene solution was dried over magnesium sulfate
  8. filtrationfiltered through diatomaceous earth
  9. customToluene was removed by high speed rotary evaporation
  10. customto yield a white solid product