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30th April 2013 @ 08:09
Mnr: mnr121-130

Using 4-bromobenzenesulfonamide as a test system as it's a lot cheaper than 3-bromobenzenesulfonamide.

As for - Synthesis of N,N-dimethyl-3-bromobenzenesulfonamide - MNR109-1

 

 

Hazard Assessment


Procedure

To a solution of 4-bromobenzenesulfonyl chloride (5.2 g, 20.35 mmol) in EtOH  (18mL) at 0 °C (THF (10 mL) was added as not all the starting material went into the EtOH solution) was added dimethylamine (33% in EtOH, 18.2 mL).  The resulting solution was allowed to warm to room temperature and stirred overnight.  In the morning TLC showed complete consumption of starting material.  The mixture was concentrated then washed with HCl (1M) (20 mL) and extracted with CHCl3 (4 x 50 mL).  The organic fractions were combined, dried, filtered and concentrated to give the crude at a off white solid.

TLC

50% EtOAc/Hexane

2013-05-01 12.19.27.jpg

 NMR

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MNR123_scheme.png
MNR123-1_table.PNG
2013-05-01 12.19.27.jpg