反应详情

A mixture of sodium hydride (0.48g.) and dimethylsulfoxide (5ml.) is stirred and heated at 70°-80° until the evolution of hydrogen ceases. The cooled solution is treated with methyltriphenylphosphonium bromide (7.14g.) in dimethylsulfoxide (10ml.), stirred for 10 minutes and treated with ethyl fluorene-2-glyoxylic acid (5.32g.). The reaction mixture is stirred for 1 hr., the solvent evaporated and the residue extracted with ether after the addition of water. The ether extracts are washed with water, dried (MgSO4) and evaporated. The residue is hydrolyzed by refluxing it in 50% methanol (50ml.) containing potassium hydroxide (5g.) for 3 hr. The reaction mixture is concentrated, acidified and extracted with ether. The ether extracts are washed with water, dried (MgSO4) and evaporated to give the title compound.

1. stirringstirred for 10 minutes
2. stirringThe reaction mixture is stirred for 1 hr
3. custom, the solvent evaporated
4. extractionthe residue extracted with ether
5. additionafter the addition of water
6. washThe ether extracts are washed with water
7. dry with materialdried (MgSO4)
8. customevaporated
9. temperatureby refluxing it in 50% methanol (50ml.)
10. additioncontaining potassium hydroxide (5g.) for 3 hr
11. concentrationThe reaction mixture is concentrated
12. extractionextracted with ether
13. washThe ether extracts are washed with water
14. dry with materialdried (MgSO4)
15. customevaporated