反应详情

A mixture of 8.4 g of 7-oxo-2,3,4,5,6,7-hexahydrobenzothiazoline-2-one, 10.5 g of potassium carbonate and 100 ml of acetone was refluxed for 1 hour and after addition of 14.5 g of O,O-diethyl chlorothiophosphate thereto, the mixture was refluxed for another hour. The mixture was stirred at room temperature for 24 hours and the mineral salts formed were filtered off. The filtrate was distilled to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with a 6 -4 cyclohexane-ethyl acetate mixture resulted in 3.5 g of 2-(diethoxythiophosphoryloxy)-4,5,6,7-tetrahydro-7-oxo-benzothiazole with a refractive index of nD20 = 1.555.

1. temperaturewas refluxed for 1 hour
2. temperaturethe mixture was refluxed for another hour
3. customthe mineral salts formed
4. filtrationwere filtered off
5. distillationThe filtrate was distilled to dryness under reduced pressure
6. customthe residue was chromatographed over silica gel
7. washElution with a 6 -4 cyclohexane-ethyl acetate mixture
8. customresulted in 3.5 g of 2-(diethoxythiophosphoryloxy)-4,5,6,7-tetrahydro-7-oxo-benzothiazole with a refractive index of nD20 = 1.555