HRID562878

反应详情

EQUATION

反应方程式

HRID 562878 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

To a 3-necked 2-L flask was added N-benzyl-N-methylethanolamine (30.5 g, 0.182 mol), DCM (0.5 L), DIPEA (95 mL, 0.546 mol) and DMSO (41 mL, 0.728 mol). Using an ice bath, the mixture was cooled to about −10° C. and sulfur trioxide pyridine-complex (87 g, 0.546 mol) was added in 4 portions over 5 minutes intervals. The reaction was stirred at −10° C. for 2 hours. Before removing the ice-bath, the reaction was quenched by adding water (0.5 L). The aqueous layer was separated and the organic layer was washed with water (0.5 L) and brine (0.5 L) and then dried over magnesium sulfate and filtered to provide the title compound which was used without further purification.

WORKUP

后处理

  1. customBefore removing the ice-bath
  2. customthe reaction was quenched
  3. additionby adding water (0.5 L)
  4. customThe aqueous layer was separated
  5. washthe organic layer was washed with water (0.5 L) and brine (0.5 L)
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered