反应详情

温度

170 °C

3-Amino-4-(2-hydroxy-2-methylpropylamino)quinoline (7.5 g, 32 mmol) was combined with methoxyacetic acid (7.5 mL, 97 mmol) and heated at about 170° C. for about 3 hours. The resulting solid residue was dissolved in ethyl acetate (150 mL). The ethyl acetate solution was extracted twice with 0.2 N sodium hydroxide, washed with water, dried over magnesium sulfate, treated with activated charcoal and then concentrated to a volume of about 50 mL. Hexane was added to the ethyl acetate and the resulting precipitate was collected and dried to provide 0.9 g of the desired product as a crystalline solid, m.p. 145-148° C. Analysis: Calculated: %C, 67.3; %H, 6.7; %N, 14.7; Found: %C, 67.2; %H, 6.6; %N, 14.6.

1. extractionThe ethyl acetate solution was extracted twice with 0.2 N sodium hydroxide
2. washwashed with water
3. dry with materialdried over magnesium sulfate
4. additiontreated with activated charcoal
5. concentrationconcentrated to a volume of about 50 mL
6. additionHexane was added to the ethyl acetate
7. customthe resulting precipitate was collected
8. customdried