Cyclohex-1-en-1-ylphosphonic acid → Cyclohexene-1-phosphonic acid dichloride
Reaction equation
C1(P(O)(=O)O)CCCCC=1.C(Cl)(Cl)=O.[C:15]1([P:21]([Cl:24])([Cl:23])=[O:22])[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]=1>>[C:15]1([P:21]([Cl:24])([Cl:23])=[O:22])[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]=1Participants
3
Procedure
Into a mixture of 57 g of cyclohexene-1-phosphonic acid and 10 g of cyclohexene-1-phosphonic acid dichloride phosgene was introduced at a temperature of from 170°-180°C for 19 hours. At the end of the reaction, nitrogen was blown through the mixture to remove excess phosgene and subsequently the mixture was distilled under reduced pressure. 62 g of cyclohexene-1-phosphonic acid dichloride were obtained, b.p. 75°C under 0.3 mm Hg, corresponding to a yield of 89.5 percent of the theory.
Workup
- additionwas introduced at a temperature of from 170°-180°C for 19 hours
- customAt the end of the reaction, nitrogen