HRID1972614

反应详情

EQUATION

反应方程式

HRID 1972614 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A 20-mL vial was charged ((2R)-1,4-dibenzyl-2-piperazinyl)methyl methanesulfonate (1.01 g, 2.70 mmol, Example 184, Step 1), aniline (1.30 mL, 14.3 mmol, Alfa Aesar, Ward Hill, Mass.) and MeOH (12 mL). The reaction mixture was sealed and heated at 140° C. for 30 min in an Initiator microwave reactor (Biotage AB, Inc., Uppsala, Sweden). The mixture was allowed to cool to room temperature and then concentrated in vacuo. The crude product was purified by column chromatography (50 g of silica gel, (2 M NH3 in MeOH) in CH2Cl2 0 to 5%) to afford N-(((2S)-1,4-dibenzyl-2-piperazinyl)methyl)aniline (0.734 g) as an orange oil.

WORKUP

后处理

  1. customThe reaction mixture was sealed
  2. temperatureto cool to room temperature
  3. concentrationconcentrated in vacuo
  4. customThe crude product was purified by column chromatography (50 g of silica gel, (2 M NH3 in MeOH) in CH2Cl2 0 to 5%)