反应详情

温度

20 °C

Thiophosphoryl chloride (17.0 g) was dissolved in toluene (250 cm3) and triethylamine (21.5 g) was added. The solution was stirred at 20° C. and 2,4-dimethylphenol (24.4 g) was added in portions during 1 hr. The mixture was stirred for 2 hr. and then heated and stirred at 80° C. for a further 2 hr. and then cooled and filtered to remove triethylamine hydrochloride. The toluene was distilled under reduced pressure leaving bis(2,4-dimethylphenyl) chlorothiophosphate (oil, 30.6 g. 31P NMR in CDCl3, singlet 54.57 ppm downfield of H3PO4).

1. stirringThe mixture was stirred for 2 hr
2. temperatureand then heated
3. stirringstirred at 80° C. for a further 2 hr
4. temperatureand then cooled
5. filtrationfiltered
6. customto remove triethylamine hydrochloride
7. distillationThe toluene was distilled under reduced pressure