反应详情

A mixture of 3-[4-methyl-3-oxo-7-(1-trifluoromethyl-vinyl)-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-ylamino]-azetidine-1-carboxylic acid tert-butyl ester (0.12 g, 0.25 mmol) and Pd/C (10%, 0.10 g, 0.1 mmol) in EtOAc (60 mL) was stirred under an atmosphere of H2 (40 psi) overnight. The mixture was filtered and the filtrate was concentrated in vacuo to give a residue which was purified by preparative TLC (eluting with 50% EtOAc in petroleum ether) to give 3-[4-methyl-3-oxo-7-(2,2,2-trifluoro-1-methyl-ethyl)-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-ylamino]-azetidine-1-carboxylic acid tert-butyl ester (0.020 g, 17%). 1H NMR (CDCl3, 400 MHz): δ 8.62 (brs, 1H), 7.29 (s, 1H), 6.97 (s, 1H), 6.97 (s, 1H), 4.72 (m, 1H), 4.53 (m, 2H), 4.33 (m, 2H), 4.11 (m, 1H), 3.77 (m, 2H), 3.63 (m, 1H), 1.50 (m, 15H).

1. filtrationThe mixture was filtered
2. concentrationthe filtrate was concentrated in vacuo
3. customto give a residue which
4. customwas purified by preparative TLC (eluting with 50% EtOAc in petroleum ether)