反应详情

温度

50 °C

A mixture was prepared by admixing, with stirring, 20 grams (g) (0.11 mole (m)) of 3,5-dichloro-6-fluoro-2-pyridinol, 16 g (0.116 m) of potassium carbonate, 0.2 g of mercuric chloride and 250 milliliters (ml) of acetonitrile. To this mixture, with stirring, was added dropwise 16 g (0.1 m) of O,O-dimethyl phosphorochloridothioate. After the addition was complete, the mixture was stirred for an additional 0.5 hour and then heated to about 50° C., with stirring, for 2 hours. The reaction mixture was cooled to room temperature and filtered to remove insolubles. The solvent was removed by evaporation under reduced pressure. The residue was dissolved in 100 ml of benzene and washed with water. The organic layer was dried and filtered. The benzene was removed by evaporation. The residue (20 g of an oil) was crystallized from 30 ml of hexane to give 13 grams of O,O-dimethyl O-(3,5-dichloro-6-fluoro-2-pyridinyl) phosphorothioate. The product, a solid, melted at room temperature and had a refractive index of nd25 =1.5370. Upon analysis, the product was found to have carbon, hydrogen and nitrogen contents of 27.40, 2.28 and 4.27 percent, respectively, as compared with the theoretical contents of 27.46, 2.31 and 4.58 percent, respectively, as calculated for the above compound.

1. customA mixture was prepared
2. stirringTo this mixture, with stirring
3. additionAfter the addition
4. stirringthe mixture was stirred for an additional 0.5 hour
5. stirringwith stirring, for 2 hours
6. temperatureThe reaction mixture was cooled to room temperature
7. filtrationfiltered
8. customto remove insolubles
9. customThe solvent was removed by evaporation under reduced pressure
10. dissolutionThe residue was dissolved in 100 ml of benzene
11. washwashed with water
12. customThe organic layer was dried
13. filtrationfiltered
14. customThe benzene was removed by evaporation
15. customThe residue (20 g of an oil) was crystallized from 30 ml of hexane