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13th March 2013 @ 02:07
Mnr: MNR101-110

Following a prep from US7235576  (B1)  -  Omega-carboxyaryl substituted diphenyl ureas as raf kinase inhibitors - page 16 column 26

Hazard Assessment

 

HIRAC MNR108.pdf

Procedure

To a solution of 3-bromobenzenesulfonyl chloride (0.20 mL, 1.37 mmol) in THF (2mL) at 0 °C was added dimethylamine (33% in EtOH, 2 mL).  The resulting solution was allowed to warm to room temperature and stirred overnight.  In the morning, HCl (1M, 5 mL) was added and the mixture was extracted with EtOAc (10 mL x 3).  The organic fractions were combined, dried, filtered and concentrated to give the crude at a off white solid (0.397 g, 110%)

 NMR

 
 
Conclusion

 

Strings

 Starting material

InChI=1S/C6H4BrClO2S/c7-5-2-1-3-6(4-5)11(8,9)10/h1-4H

Product

InChI=1S/C8H10BrNO2S/c1-10(2)13(11,12)8-5-3-4-7(9)6-8/h3-6H,1-2H3

Linked Posts
Attached Files
MNR109_scheme.png
MNR109-1_table.PNG
HIRAC MNR108.pdf