反应详情

A solution of (3-ethyl-5-methylisoxazol-4-yl)-carbamic acid 2-trimethylsilanylethyl ester (1.8 g) in tetrabutylammonium fluoride (26.7 ml of a 1.0M solution in tetrahydrofuran) was heated at 50° C. for 30 mins. The solvent was removed in vacuo and the residue dissolved in ethyl acetate (150 ml), washed with sodium hydrogencarbonate solution (30 ml), washed with water (30 ml) and washed with brine (30 ml). The organic layer was separated, dried over magnesium sulphate, filtered and the solvent removed in vacuo. Purification by column chromatography on silica eluting with 50-100% ethyl acetate in hexane afforded the title compound as a yellow oil (0.35 g).

1. customThe solvent was removed in vacuo
2. dissolutionthe residue dissolved in ethyl acetate (150 ml)
3. washwashed with sodium hydrogencarbonate solution (30 ml)
4. washwashed with water (30 ml)
5. washwashed with brine (30 ml)
6. customThe organic layer was separated
7. dry with materialdried over magnesium sulphate
8. filtrationfiltered
9. customthe solvent removed in vacuo
10. customPurification by column chromatography on silica eluting with 50-100% ethyl acetate in hexane