HRID437188

反应详情

EQUATION

反应方程式

HRID 437188 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Hydroxymethyl-4-n-propylmorpholine (16.2 g.) is dissolved in dry pyridine (50 ml.) and a solution of toluene-p-sulphonylchloride (21.4 g.) in dry pyridine (50 ml.) is added dropwise with stirring. The mixture is stirred at 20°-25° C. for 3 hours. The pyridine is removed under reduced pressure, water (100 ml.) is added to the residue and the product is extracted into ether (3× 150 ml.). The ethereal solution is washed with water, dried (MgSO4), filtered and the ether evaporated to give 4-n-propyl-2-toluene-p-sulphonyloxymethylmorpholine (30.6 g.) as an oil which forms a hydrochloride, m.p. 172°-173° C. on recrystallisation from methanol/ether.

WORKUP

后处理

  1. stirringThe mixture is stirred at 20°-25° C. for 3 hours
  2. customThe pyridine is removed under reduced pressure, water (100 ml.)
  3. additionis added to the residue
  4. extractionthe product is extracted into ether (3× 150 ml.)
  5. washThe ethereal solution is washed with water
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customthe ether evaporated