反应详情

温度

56 °C

5-(2,6-Diethoxy-4′-methoxymethoxy-biphenyl-4-ylmethyl)-pyrimidine-2,4-diamine (10.06 g; 23.7 mmol) is dissolved in methanol (410 ml), and a 3 N hydrochloric acid solution in methanol (119.1 ml; 357.3 mmol) is added. The reaction mixture is stirred for 30 minutes at a temperature of 56° C. and concentrated. The grey residue is then stirred with water (400 ml), the pH is brought to 9 by addition of an aqueous saturated ammonia solution (approx. 8 ml) and the entire mixture is stirred for 15 minutes. The greyish suspension is filtered with suction and the residue is dried under a high vacuum. 8.85 g (98%) 4′-(2,4-diamino-pyrimidin-5-ylmethyl)-2′,6′-diethoxy-biphenyl-4-ol are obtained as a greyish powder.

1. concentrationconcentrated
2. stirringThe grey residue is then stirred with water (400 ml)
3. additionthe pH is brought to 9 by addition of an aqueous saturated ammonia solution (approx. 8 ml)
4. stirringthe entire mixture is stirred for 15 minutes
5. filtrationThe greyish suspension is filtered with suction
6. customthe residue is dried under a high vacuum