反应详情

Sodium hydride (170 mg, 80% dispersion in oil) was added to a solution of trans-6-cyano-3,4-dihydro-2,2-dimethyl-4-(2-oxo-1-piperidinyl)-2H-1-benzopyran-3-ol (1.65 g) in anhydrous tetrahydrofuran (25 ml) and the reaction mixture stirred and heated under reflux for 48 hours. Work up as in Example 1, followed by chromatography (chromatotron--2 mm Silica gel HF254 --elution with ethyl acetate at 6 ml/min) gave one fraction (312 mg) which on recrystallisation from ethyl acetate gave the title compound as crystals (66 mg) of m.p. 162°-163° C.

1. temperatureheated
2. temperatureunder reflux for 48 hours
3. washWork up as in Example 1, followed by chromatography (chromatotron--2 mm Silica gel HF254 --elution with ethyl acetate at 6 ml/min)
4. customgave one fraction (312 mg) which
5. customon recrystallisation from ethyl acetate