Reaction #2186168

Reaction equation

2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octanol

phosphorus oxychloride

triethylamine

→

[2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octyl] dichlorophosphate

Yield 34.7%

Solvents

toluene

Conditions

Workup

1. 1
   Otherthe mixture was reacted for 12 hours at 0 degrees C
2. 2
   TemperatureThe mixture was then heated to 25 degrees C
3. 3
   Other, and a triethylamine hydrochloride was removed
4. 4
   Filtrationby filtering

Procedure

With nitrogen substitution, 540 ml of toluene and 138.0 grams (0.9 moles) of phosphorus oxychloride were added and cooled to −10 degrees C. To this mixture, a solution of 243.5 grams (0.9 moles; 1.0 in molar ratio) of 2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octanol and 91.1 grams (0.9 moles) of triethylamine was dripped, and the mixture was reacted for 12 hours at 0 degrees C. The mixture was then heated to 25 degrees C., and a triethylamine hydrochloride was removed by filtering to obtain 1003.9 grams of a toluene solution of [2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octyl] dichlorophosphate (34.7% in concentration).

Source