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4th April 2013 @ 06:09
Mnr: MNR111-120

Microwave Assisted Arylation of MNR115-2 using MNR103-1 to give MNR120-1

Starting material from Bromination of MNR113-1 to give MNR115-2

and Synthesis of Boronic Acid Pinacol Ester - MNR103-1

as for Arylation of aminobromothienopyrimidine (AT-17-1)

Hazard Assessment

 

 

 

Procedure

MNR115-2 (0.07 g, 0.17 mmol), MNR103-1 (0.058 g, 0.21 mmol) and PdCl2(dppf) (0.025 g, 0.03 mmol) were added to a microwave tube and added was IPA (2 ml) and potasisium carbonate solution (1M) (0.34 ml, 0.34 mmol).  The mixture was degassed with argon for 5 mniutes then sealed and heated to 90 °C in the microwave reactor (200 W) for 30 minutes. 

 

NMR

 

mnr120-1_1H.pdf
mnr120-1.zip

Conclusion

good 1H NMR, sample can be sent for testing

Strings

Starting material

InChI=1S/C12H18BNO4S/c1-11(2)12(3,4)18-13(17-11)9-6-5-7-10(8-9)19(14,15)16/h5-8H,1-4H3,(H2,14,15,16)

InChI=1S/C17H16BrFN4S/c18-15-9-14-16(24-15)17(21-11-20-14)23-7-5-22(6-8-23)10-12-1-3-13(19)4-2-12/h1-4,9,11H,5-8,10H2

Product

InChI=1S/C23H22FN5O2S2/c24-18-6-4-16(5-7-18)14-28-8-10-29(11-9-28)23-22-20(26-15-27-23)13-21(32-22)17-2-1-3-19(12-17)33(25,30)31/h1-7,12-13,15H,8-11,14H2,(H2,25,30,31)

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Attached Files
MNR120-1_table.PNG
MNR120_scheme.png
mnr120-1_1H.pdf
mnr120-1.zip