반응 #68888

반응 방정식

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

용매

DMF

반응 조건

후처리

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

실험 절차

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).

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