تفاعل #2458

معادلة التفاعل

Thiophosphoryl chloride

2,4-dimethylphenol

→

bis(2,4-dimethylphenyl) chlorothiophosphate

المردود 89.9%

المذيبات

triethylamine

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر