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1st March 2013 @ 10:23

 

The product from the previous step Amination of PT-1-4 (PT-1-9) (42.1 mg 118 umol), was suspended in MeOH (10 ml) and saturated aqueous ammonia (10 ml) and stirred for 1 hour, whereupon TLC (PT-1-10-A1) indicated completion (ca. 90% pure by NMR, PT-1-10-B1). The reaction was concentrated in vacuo and purified by dry column vacuum chromatogrphy (gradient: 50-100% ethyl acetate, background heptane, 6 fractions, then ethyl acetate, 6 fractions) to give the desired product as a white foam (28.1 mg, 82 umol, 69%).

 

Analysis:

PT-1-10-C1 MS nominal.jpg
PT-1-10-C1 NMR 1H.pdf
PT-1-10-C1 NMR 13C.pdf






Mass spectroscopy: ESI-NOM found 362.0 [M+Na]+, 700.6 [2M + Na]+.

ESI-Acc (Finnegan MAT-900 ESI-Positive HRMS): Expected 339.10474 (C15H18O3N3FS) Found 339.10460 (0.14 ppm)

 

NMR Spectroscopy: Consistent with expected product.

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Attached Files
PT-1-10.png
PT-1-10-A1 TLC.jpg
PT-1-10-B1 NMR.pdf
PT-1-10-C1 MS nominal.jpg
PT-1-10-C1 NMR 13C.pdf
PT-1-10-C1 NMR 1H.pdf
ThomsonPatrick_ptm110c1_010313_1H-13C_av500.tar