Реакция #68888

Уравнение реакции

MeI

4-(3,4-dibromo-benzyl)-piperazine-1-carboxylic acid phenylamide

NaH

→

product

4-(3,4-Dibromo-benzyl)-piperazine-1-carboxylic acid methyl-phenyl-amide

Растворители

DMF

Условия реакции

Обработка

1. 1
   workup.STIRRINGwas stirred at rt for 12 h
2. 2
   КонцентрированиеThe mixture was concentrated
3. 3
   Другоеthe residue was purified by column chromatography (5% MeOH/DCM)

Методика

To a solution of 4-(3,4-dibromo-benzyl)-piperazine-1-carboxylic acid phenylamide (0.02 g) in DMF (0.6 mL) was added NaH (60% dispersion in oil; 3 mg) in one portion. The resulting mixture was allowed to stir for 30 min, then was treated with MeI (0.005 mL), and was stirred at rt for 12 h. The mixture was concentrated and the residue was purified by column chromatography (5% MeOH/DCM), giving the product as a white solid (0.015 g). 1H NMR (400 MHz, CDCl3): 7.54-7.50 (m, 2H), 7.33-7.31 (m, 2H), 7.12-7.05 (m, 4H), 3.34 (s, 2H), 3.22-3.20 (m, 6H), 2.23-2.21 (m, 4H), 1.63 (s, 3H).

Источник