Propylene Glycol → 2-Trichloromethyl-[1,3]dioxane

HRID 1196745Notes

Reaction equation

HRID 1196745 reaction equation
[Cl:1][C:2]([Cl:7])([Cl:6])[CH:3]([OH:5])[OH:4].[CH2:8](O)[CH:9](O)[CH3:10].S(=O)(=O)(O)O>>[Cl:1][C:2]([Cl:7])([Cl:6])[CH:3]1[O:5][CH2:10][CH2:9][CH2:8][O:4]1

Participants

4

Reactant 3

HCID 1030Propylene GlycolHCID 1118Sulfuric AcidHCID 2707Chloral Hydrate

Product 1

HCID 2682362-Trichloromethyl-[1,3]dioxane

Procedure

21.6 g of chloral hydrate are admixed with 9.6 g of propylene-glycol, then 16.8 ml of concentrated sulphuric acid are added. It is heated at 60°-70° C. for two hours and after dilution with 60 ml of water it is extracted two times with 60 ml of chloroform. The chloroformic phase is washed with water and sodium hydrogen carbonate, dried on magnesium sulfate, then the product is vacuum distilled after distilling off the chloroform.

Workup

  1. temperatureIt is heated at 60°-70° C. for two hours
  2. extractionafter dilution with 60 ml of water it is extracted two times with 60 ml of chloroform
  3. washThe chloroformic phase is washed with water and sodium hydrogen carbonate
  4. customdried on magnesium sulfate
  5. distillationdistilled
  6. distillationafter distilling off the chloroform

Sources & evidence

ORD record
ord-5b9d9a7a162e44aa88775f260dcd6d8a
Source dataset
uspto-grants-1992_05
Patent number
US05116402

Reaction notes

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