Hydrochloric Acid → HCID 54554324, compound

HRID 1730250Notes

Reaction equation

HRID 1730250 reaction equation
I[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[Cl:8].[CH3:9][P:10]([O:14]CC)[O:11]CC.Cl>>[Cl:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[P:10]([CH3:9])(=[O:11])[OH:14]

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 119931-Chloro-2-iodobenzeneHCID 85063Diethyl methylphosphonite

Product 1

HCID 54554324HCID 54554324, compound

Procedure

After dissolving 4.8 grams of o-iodochlorobenzene in 10 ml. of diethyl methylphosphonite, the resulting solution is irradiated for 3 hours. After concentration under reduced pressure and vacuum distillation, a colorless oil is produced having a boiling point from 96°-100° C. (0.05- 0.1 mm. Hg.). The product is combined with 25 ml. of 12M HCl, and the mixture is refluxed for 2 hours. The solution is concentrated to leave a thick oil which crystallizes upon trituration with ether. Upon recrystallization from acetone-ether, 0.5 grams of the solid is collected having a melting point of 97°-98° C.

Workup

  1. concentrationAfter concentration
  2. distillationunder reduced pressure and vacuum distillation
  3. customa colorless oil is produced
  4. customfrom 96°-100° C.
  5. concentrationThe solution is concentrated
  6. customto leave a thick oil which
  7. customcrystallizes upon trituration with ether
  8. customUpon recrystallization from acetone-ether, 0.5 grams of the solid
  9. customis collected

Sources & evidence

ORD record
ord-79f0eaa0a6fb4e51ba35e43efd9f4aa4
Source dataset
uspto-grants-1976_11
Patent number
US03992273

Reaction notes

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