Réaction #2458

Équation de réaction

Thiophosphoryl chloride

2,4-dimethylphenol

→

bis(2,4-dimethylphenyl) chlorothiophosphate

Rendement 89.9%

Solvants

triethylamine

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGThe mixture was stirred for 2 hr
3. 3
   Températureand then heated
4. 4
   workup.STIRRINGstirred at 80° C. for a further 2 hr
5. 5
   Températureand then cooled
6. 6
   Filtrationfiltered
7. 7
   Autreto remove thriethylamine hydrochloride
8. 8
   workup.DISTILLATIONThe toluene was distilled under reduced pressure

Mode opératoire

Thiophosphoryl chloride (17.0 g) was dissolved in tuoluene (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 thriethylamine 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 H3 PO4).

Source