Pyridine → HCID 53712289, compound

HRID 2163794

Reaction equation

HRID 2163794 reaction equation
[CH2:1]([OH:4])[CH:2]=[CH2:3].[Cl:5][CH2:6][CH2:7][P:8](Cl)(Cl)=[O:9].N1C=C[CH:15]=[CH:14][CH:13]=1.CC[O:20]CC>>[Cl:5][CH2:6][CH2:7][P:8]([O:9][CH2:13][CH:14]=[CH2:15])(=[O:20])[O:4][CH2:1][CH:2]=[CH2:3]

Participants

5

Reactant 4

HCID 1049PyridineHCID 3283Diethyl EtherHCID 7858Allyl AlcoholHCID 69645(2-Chloroethyl)phosphonic dichloride

Product 1

HCID 53712289HCID 53712289, compound

Procedure

To a solution of 11.6 g (0.2 mol) of allyl alcohol and 18.1 g (0.1 mol) of 2-chloroethane phosphonic acid dichloride in 150 ml of absolute ether are added dropwise with stirring 15.8 g (0.2 mol) of pyridine. When the exothermic reaction is complete, stirring is continued for 15 hours at 40° after which the precipitated hydrochloride is removed by filtration and the ethereal filtrate washed to neutrality with water, dried and then evaporated. It is further dried by rotation under high vacuum over a period of 2 hours at 25°. A yellowish oil is obtained having the following characterisation data:

Workup

  1. customWhen the exothermic reaction
  2. customafter which the precipitated hydrochloride is removed by filtration
  3. washthe ethereal filtrate washed
  4. customdried
  5. customevaporated
  6. customIt is further dried by rotation under high vacuum over a period of 2 hours at 25°
  7. customA yellowish oil is obtained

Sources & evidence

ORD record
ord-73bbe8295ddd41c084492d156b3efa8f
Source dataset
uspto-grants-1979_01
Patent number
US04137064

Linked notes

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