HRID1972614
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction mixture was sealed
- temperatureto cool to room temperature
- concentrationconcentrated in vacuo
- customThe crude product was purified by column chromatography (50 g of silica gel, (2 M NH3 in MeOH) in CH2Cl2 0 to 5%)