反应详情

5-Carbamoyl-4-[2-(2-isopropyl-2H[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diaza-benzo[e]azulen-8-yl]-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester was stirred in TFA (1 mL) and DCM (2 mL) for 2 h. The reaction mixture was concentrated in vacuo and the residue triturated with diethyl ether to give a solid. The solid was then treated with tetra allylammonium carbonate (polymer bound) (1.84 g, 4.68 mmol) in methanol and DCM for 30 min. The resin was filtered off and the filtrate concentrated in vacuo to give 4-[2-(2-Isopropyl-2H[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diaza-benzo[e]azulen-8-yl]-1,2,5,6-tetrahydro-pyridine-3-carboxylic acid amide (0.40 g, 82%). 1H NMR 300 MHz (CDCl3) δ: 8.52-8.46 (1H, m), 7.88 (1H, s), 7.71-7.69 (1H, m), 7.08 (1H, dd, J=8.30, 1.82 Hz), 6.98 (1H, d, J=1.79 Hz), 6.01-6.00 (1H, m), 4.52-4.47 (4H, m), 3.75 (2H, s), 3.15 (2H, t, J=5.82 Hz), 2.51 (2H, m), 1.60 (6H, d, J=6.62 Hz).

1. concentrationThe reaction mixture was concentrated in vacuo
2. customthe residue triturated with diethyl ether
3. customto give a solid
4. filtrationThe resin was filtered off
5. concentrationthe filtrate concentrated in vacuo