反应详情

温度

65 °C

50 G. of 2-ethyl-4-amino-5-methoxymethyl pyrimidine, 50 g. of 7-methylthieno[2,3-c]pyridine and 500 ml. of xylene are placed in a 2-liter flask equipped with reflux condenser, stirrer, thermometer and gas inlet tube. Hydrogen chloride gas is added to this mixture over 30 minutes at a rate sufficient to add an amount equivalent to 0.2 moles, that of the pyrimidine. The temperature rises to about 67° C. The gas inlet tube is replaced with a distillation unit and the mixture heated at reflux (138° C.) for two hours during which fresh xylene is added to replace the volume of liquid that distills. An additional 25 g. of 7-methylthieno[2,3-c]pyridine are added and the mixture refluxed for 40 minutes. At the end of the reflux period, the reaction mixture is cooled to 65° C., the xylene decanted, and 50 ml. of acetonitrile added to the residue. The resulting mixture is stirred at room temperature for about 12 hours, filtered, and the solid 6-[(4-amino-2-ethyl-5-pyrimidinyl)methyl]-7-methylthieno-[2,3-c]pyridinium chloride hydrochloride thus obtained washed. The product has a m.p. of 249°-250° C., dec.

1. customequipped
2. temperaturewith reflux condenser, stirrer
3. additionto add an amount equivalent to 0.2 moles
4. customrises to about 67° C
5. temperaturethe mixture heated
6. additionis added
7. distillationthat distills
8. additionof 7-methylthieno[2,3-c]pyridine are added
9. temperaturethe mixture refluxed for 40 minutes
10. customthe xylene decanted
11. additionof acetonitrile added to the residue
12. filtrationfiltered