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26th March 2013 @ 15:13

 

PT-1-11A (16.6 mg 48.8 umol), was suspended in MeOH (10 ml) and saturated aqueous ammonia (10 ml) and stirred for 30 minutes, whereupon TLC indicated completion. The reaction was concentrated in vacuo to give a solid which was purified the same way as Amidation of PT-1-9A (PT-1-10) then dried in vacuo to give a white solid PT-1-12-C1 (7 mg, 21 umol, 43%, Rf 0.55 (ethyl acetate)). 

 

Analysis: NMR consistent with Amidation of PT-1-9A (PT-1-10), sans N-methyl group and introduction of an N-H at 5.1 ppm, plus traces of ethyl acetate. Mass spec consistent (ESI-Nom).

ESI-Acc (Finnegan MAT-900 ESI-Positive HRMS): Expected 325.08909 (C14H16O3N3FS) Found 325.08881 (0.28 ppm)

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Attached Files
PT-1-12.png
PT-1-12-B1.pdf
PT-1-12-C1 1H.pdf
PT-1-12-C1 13C.pdf
ThomsonPatrick_ptm112c1_270313_1H-13C_av500.tar
PT-1-12-C1 MS.jpg