反应详情

4.4 g (13.27 mmol) of 6,7-bis(3-hydroxyphenyl)-pteridin-4-ylamine was suspended in 35 ml of MeOH. A solution of 2.61 g of aq. HCl (26.55 mmol, 12.1 N) in 5 mL of MeOH was added to the suspension. The reaction mixture became homogeneous within 5 min of stirring. It was left to stir for 30 min and then added dropwise to 400 mL of diethyl ether with vigorous stirring. The resulting precipitate was collected, washed repeatedly with ether and dried in vacuo to give 4.62 g (94.7% yield) of the product as a bright-yellow solid. 98.3% purity by LC/MS (230 DAD). Mass-spec [ES+]=332.8. 1H NMR (MeOH) 6.88–6.90 (2H, m), 6.99–7.02 (2H, m), 7.04–7.08 (2H, m), 7.17–7.20 (2H, m), 8.79 (1H, s).

1. waitIt was left
2. stirringto stir for 30 min
3. customThe resulting precipitate was collected
4. washwashed repeatedly with ether
5. customdried in vacuo