反应详情

A suspension of 7-[3-[N-benzyl,N-(3-nicotinylpropyl)amino]-2-hydroxypropoxy]flavone (4.50 g, 8.64 mmol), Example 17b, palladium black (0.1 g), cyclohexene (30 ml), and acetic acid (30 ml) was refluxed for 6 hours. The solvent was evaporated to give a residue which was dissolved in water and washed with chloroform (twice) to remove impurities. The aqueous solution was basified with 2.5N NaOH and then extracted with methylene chloride several times. The extracts were washed with water, dried (MgSO4), and evaporated to afford a yellow solid of 2.9 g. Recrystallization from isopropyl alcohol gave light yellow crystals (2.0 g; 54% yield), mp 116°-119° C.

1. temperaturewas refluxed for 6 hours
2. customThe solvent was evaporated
3. customto give a residue which
4. washwashed with chloroform (twice)
5. customto remove impurities
6. extractionextracted with methylene chloride several times
7. washThe extracts were washed with water
8. dry with materialdried (MgSO4)
9. customevaporated
10. customto afford a yellow solid of 2.9 g
11. customRecrystallization from isopropyl alcohol
12. customgave light yellow crystals (2.0 g; 54% yield), mp 116°-119° C.