HRID1170474

反应详情

EQUATION

反应方程式

HRID 1170474 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

2-(Methylamino)ethanol (22.0 g, 290 mmol) is added all at once to a stirred solution of 3,4-methylenedioxybenzyl chloride (25.0 g, 147 mmol) in DCM (45 mL) at −78° C. under nitrogen. The solution is stirred for 15 minutes at −78° C. then allowed to warm to room temperature overnight (16 h). The reaction is quenched with 1.2 M NaOH (100 mL), washed twice with water, dried of MgSO4, and filtered. Concentration under reduced pressure afforded 25.3 g (83%) of 2-(benzo[1,3]dioxol-5-ylmethyl-methyl-amino)-ethanol as a clear oil which was suitable for use in the next step.

WORKUP

后处理

  1. temperatureto warm to room temperature overnight (16 h)
  2. customThe reaction is quenched with 1.2 M NaOH (100 mL)
  3. washwashed twice with water
  4. dry with materialdried of MgSO4
  5. filtrationfiltered
  6. concentrationConcentration under reduced pressure