反应详情

Sodium Hydroxide (0.66 g; 16.5 mmol) was added to a suspension of 2-amino-4-phenyl-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (Example 1) (1.00 g; 3.34 mmol) in ethanol (20 ml) and water (2 ml). The mixture was heated at reflux for 1 hour (affording a homogeneous pale-yellow solution) and allowed to cool to ambient temperature. Solvents were removed in vacuo and the solid residue was dissolved in water (30 mL) and cooled with ice-water bath. The mixture was stirred and adjusted to pH 1-2 by drop-wise addition of concentrated Hydrochloric acid. The resulting precipitate was filtered, washed with water, then ethanol and finally diethyl ether. The off-white product was dried in vacuo to afford 2-amino-4-phenyl-thieno[2,3-d]pyrimidine-6-carboxylic acid as a colourless solid (0.784 g; 87%).

1. temperatureThe mixture was heated
2. temperatureat reflux for 1 hour (
3. customaffording a homogeneous pale-yellow solution) and
4. customSolvents were removed in vacuo
5. dissolutionthe solid residue was dissolved in water (30 mL)
6. temperaturecooled with ice-water bath
7. additionadjusted to pH 1-2 by drop-wise addition of concentrated Hydrochloric acid
8. filtrationThe resulting precipitate was filtered
9. washwashed with water
10. customThe off-white product was dried in vacuo