反应详情

31.2 mg (0.1 mmol) of 2-amino-4-[4-(2-hydroxyethoxy)phenyl]-6-sulphanyl-pyridine-3,5-dicarbonitrile are dissolved in 0.3 ml of DMF. 33.6 mg (0.4 mmol) of sodium bicarbonate and 26.7 mg (0.15 mmol) of 4-methyl-2-chloro-1,3-thiazole hydrochloride are then added. The suspension is shaken at RT overnight, filtered, and purified by preparative HPLC [column: Macherey-Nagel VP 50/21 Nucleosil 100-5 C18 Nautilus, 20×50 mm; flow rate: 25 ml/min; gradient (A=acetonitrile, B=water+0.3% trifluoroacetic acid): 0 min 10% A; 2.0 min 10% A; 6.0 min 90% A; 7.0 min 90% A; 7.1 min 10% A; 8.0 min 10% A; detection: 220 nm]. Concentration of the appropriate fraction gives 20.2 mg (47.7% of theory) of product.

1. filtrationfiltered
2. custompurified by preparative HPLC [column
3. custom0 min 10% A
4. custom2.0 min 10% A
5. custom6.0 min 90% A
6. custom7.0 min 90% A
7. custom7.1 min 10% A
8. custom8.0 min 10% A
9. customConcentration of the appropriate fraction gives 20.2 mg (47.7% of theory) of product