反应详情

A stirred solution of 4 gms of 2-[2-[(2-nitrophenyl)methyl]-3-thienyl]-1,3-dioxolane in acetone (50 ml) and acetic acid (90% 50 ml) is heated to 60° C. Zinc dust (10 gms) is slowly added and after the addition, reaction mixture is stirred for 6 hours. At the end, reaction mixture is filtered and the residue washed with acetone and concentrated. The brown residue is extracted with chloroform and washed well with water. The organic layer is dried (Na2SO4) and filtered and concentrated. The product is isolated by silica gel column chromatography by eluting with 20% ethyl acetate:hexane to give 2.0 g of the desired product as a pale yellow crystalline solid, m.p. 86° C. Mass Spectrum; M+ 202.

1. additionafter the addition, reaction mixture
2. customAt the end, reaction mixture
3. filtrationis filtered
4. washthe residue washed with acetone
5. concentrationconcentrated
6. extractionThe brown residue is extracted with chloroform
7. washwashed well with water
8. dry with materialThe organic layer is dried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated
11. customThe product is isolated by silica gel column chromatography
12. washby eluting with 20% ethyl acetate