Carbon Tetrachloride → HCID 20087058, compound

HRID 1608692Notes

Reaction equation

HRID 1608692 reaction equation
[CH:1]([CH:4]1[O:9][CH2:8][CH:7]([CH2:10]O)[CH2:6][O:5]1)([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:32]>>[CH:1]([CH:4]1[O:9][CH2:8][CH:7]([CH2:10][Cl:32])[CH2:6][O:5]1)([CH3:3])[CH3:2]

Participants

4

Reactant 3

HCID 5943Carbon Tetrachloride2×HCID 11776TriphenylphosphineHCID 38684535113-53-2

Product 1

HCID 20087058HCID 20087058, compound

Conditions

Temperature
70 °C

Procedure

A solution of 217 g 2-isopropyl-5-hydroxymethyl-1,3-dioxane in 11 of carbon tetrachloride is added dropwise to a solution of 356 g triphenylphosphine in 1 l of carbon tetrachloride, heated to 70° C. The mixture is refluxed and after approx. 1 hour cooled down (ice-bath), filtrated and evaporated. The residue is repeatedly treated with diethylether and filtered. After evaporating the filtrate the residue is purified by distillation. The desired 2-isopropyl-5-chloromethyl-1,3-dioxane is obtained as a colorless liquid; b.p. 84°-94° C. mm Hg; cis-trans mixture; identification by NMR.

Workup

  1. temperatureThe mixture is refluxed and after approx. 1 hour
  2. temperaturecooled down (ice-bath)
  3. filtrationfiltrated
  4. customevaporated
  5. additionThe residue is repeatedly treated with diethylether
  6. filtrationfiltered
  7. customAfter evaporating the filtrate the residue
  8. distillationis purified by distillation

Sources & evidence

ORD record
ord-3bdd933d53ad4c0aa4b03b827a227172
Source dataset
uspto-grants-1995_03
Patent number
US05395946

Reaction notes

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