反应详情

A stirred mixture of 7.0 g (0.0157 mole) of the 2,4-bis(1-n-propyl-2-methyl-3-indolyl)-4-oxobutanoic acid prepared as described in A above, 2.7 g (0.017 mole) of 1-ethyl-2-methylindole, 100 ml of acetic anhydride and 1.0 ml of glacial acetic acid was aerated by bubbling air through the mixture for approximately eight hours at a temperature in the range of 48°-52° C. The solid that formed was collected by filtration. A second crop of product was obtained by drowning the filtrate in a stirred mixture of ice, benzene and sufficient concentrated ammonia hydroxide to make the mixture slightly alkaline. The benzene layer was separated, dried over molecular sieves, filtered and the filtrate set aside for several hours. The crystals, which separated from the solution, were collected by filtration and combined with the first crop of product. The combined solids were dried in vacuo at 60° C. to obtain 3,5-bis-(1-n-propyl-2-methyl-3-indolyl)-5-(1-ethyl-2-methyl-3-indolyl)-2(5H)-furanone (Formula III: R=CH3CH2CH2 ; R1 =R3 =CH3 ; R2 =CH3CH2 ; Y=Y1 =H) as a tan solid which decomposed at 179° C.

1. customprepared
2. customby bubbling air through the mixture for approximately eight hours at a temperature in the range of 48°-52° C
3. customThe solid that formed
4. filtrationwas collected by filtration
5. customA second crop of product was obtained
6. customThe benzene layer was separated
7. customdried over molecular sieves
8. filtrationfiltered
9. waitthe filtrate set aside for several hours
10. customThe crystals, which separated from the solution
11. filtrationwere collected by filtration
12. customThe combined solids were dried in vacuo at 60° C.