反应详情

2.66 g (7.68 mmol) of 6,7-bis(3-hydroxyphenyl)-pteridine-2,4-diamine was added to a solution of 1.55 g (16.13 mmol) of methanesulfonic acid in 20 mL of MeOH with stirring. Pteridine immediately dissolved to give a dark-greenish solution. The reaction mixture was stirred for 30 min and then added dropwise to 400 mL of diethyl ether with vigorous stirring. The formed yellow precipitate was collected, washed repeatedly with ether and dried in vacuo to give 3.36 g (99.1% yield) of the product as a light-yellow powder. 95.5% purity by LC/MS (230 DAD). Mass-spec [ES+]=347. 1H NMR (MeOH-d4) 2.71 (3H, s), 6.80–6.85 (2H, m), 6.90–6.92 (2H, m), 6.95 (1H, m), 7.00 (1H, m), 7.12–7.16 (2H, m).

1. customto give a dark-greenish solution
2. stirringThe reaction mixture was stirred for 30 min
3. customThe formed yellow precipitate was collected
4. washwashed repeatedly with ether
5. customdried in vacuo