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25th March 2013 @ 04:30
Mnr: MNR81-90

Synthesis of thienopyrimidine (MNR89-2) from methyl-3-aminothiophene-2-carboxylate

As for Synthesis of thienopyrimidine MNR89-1

Synthesis of thienopyrimidine MNR89-2

Hazard Assessment

HIRAC MNR89.pdf

Procedure

To methyl-3-aminothiophene-2-carboxylate (13.59 g, 86.46 mmol) and ammonium formate (6.0 g, 95.1 mmol) was added formic acid (3.59 mL, 95.1 mmol) and formamide (18.89 mL, 475 mmol) and the mixture was heated to 140 °C.  After 15 hours the reaction was cooled to room temperature and a solid formed.  This was washed with water and filtered to give an off white solid. The crude was recrystalised with EtOH (400 ml) to give fine white crystals.

 

NMR

mnr89-3_filter_1H.pdf
mnr89-3_filter_13C.pdf
mnr89-3_filter.zip
 

Conclusion


Strings


Starting Material

InChI=1S/C6H7NO2S/c1-9-6(8)5-4(7)2-3-10-5/h2-3H,7H2,1H3

InChI=1S/CH3NO/c2-1-3/h1H,(H2,2,3)

Product

InChI=1S/C6H4N2OS/c9-6-5-4(1-2-10-5)7-3-8-6/h1-3H,(H,7,8,9)

Linked Posts
Attached Files
MNR89-3_table.PNG
mnr89-3_filter_1H.pdf
mnr89-3_filter_13C.pdf
mnr89-3_filter.zip