反应详情

温度

40 °C

A solution of 1-(9H-fluoren-9-ylmethoxycarbonyl amino)-cyclohexanecarboxylic acid (0.326 g, 0.9 mmol) in pyridine (1 mL) and DMF (1 ml) was heated to 40° C. for 30 min. Carbonyl diimidazole (0.15 g, 0.9 mmol) was added and the mixture was stirred at 40° C. for 1 hour then treated with 2,3-diamino-benzamide dihydrochloride (prepared as described in WO0026192, 0.2 g, 0.9 mmol). After stirring for 1 hour at room temperature, isopropyl alcohol (3 ml) was added and the solution was cooled overnight at 0° C. The precipitated solid was filtered, dissolved in water (3 ml), treated with 50% aqueous NaOH (0.071 ml) then stirred for 3 hours at room temperature. The mixture was filtered and used immediately in Example 48B.

1. stirringAfter stirring for 1 hour at room temperature
2. temperaturethe solution was cooled overnight at 0° C
3. filtrationThe precipitated solid was filtered
4. dissolutiondissolved in water (3 ml)
5. additiontreated with 50% aqueous NaOH (0.071 ml)
6. stirringthen stirred for 3 hours at room temperature
7. filtrationThe mixture was filtered