反应详情

A solution of 2-[(4-amino-pyrrolo[2,1-f][1,2,4]triazin-7-yl)-hydroxy-methyl]-cyclopropanecarboxylic acid ethyl ester (1.75 g, 6.3 mmol) in dichloromethane (17.5 mL) was added dropwise into a mixture of triethylsilane (3 g, 25 mmol) and TFA (17.5 mL) in ice water bath. It was stirred at rt for overnight. 2N sodium carbonate solution (10 mL) was added and organic layer was separated, dried and concentrated. The residue was purified by Biotage® to give desired product 0.43 g (26). 1H NMR (300 MHz, DMSO-d6) δ 8.80 (s, 1 H), 8.75 (bs, 2 H), 6.80 (s, 1 H), 6.60 (m, 1 H), 4.0 (m, 2 H), 2.9 (d, 2 H), 1.5 (m, 2 H), 1.2 (t, 3 H), 1.0 (m, 2 H); ES-MS m/z 261.07 [M+H]+, HPLC RT (min) 2.03.

1. customorganic layer was separated
2. customdried
3. concentrationconcentrated
4. customThe residue was purified by Biotage®