Hydrochloric Acid → Dimethylmalonyl Dichloride

HRID 258971

Reaktionsgleichung

Reaktionsgleichung von HRID 258971
[CH3:1][C:2]([CH3:9])([C:6](O)=[O:7])[C:3](O)=[O:4].S(Cl)([Cl:12])=O.[ClH:14].S(=O)=O>>[CH3:1][C:2]([CH3:9])([C:6]([Cl:12])=[O:7])[C:3]([Cl:14])=[O:4]

Komponenten

5

Versuchsvorschrift

To a 500 ml. one-necked flask equipped with reflux condenser with drying tube, is added 50 grams (0.38 mole) dimethylmalonic acid (Aldrich Chemical Co.) and 300 ml. thionyl chloride. The mixture is heated to reflux for about 1 hour during which time the dimethylmalonic acid is dissolved and hydrogen chloride and sulfur dioxide are evolved. The unreacted thionyl chloride is removed by distillation under reduced pressure. The residue is recrystallized twice from cyclohexane to yield a white solid, M.P. 186°-187° C.

Aufarbeitung

  1. customone-necked flask equipped
  2. temperaturewith reflux condenser
  3. customwith drying tube
  4. temperatureThe mixture is heated
  5. dissolutionis dissolved
  6. customThe unreacted thionyl chloride is removed by distillation under reduced pressure
  7. customThe residue is recrystallized twice from cyclohexane
  8. customto yield a white solid, M.P. 186°-187° C.

Quellen und Nachweise

ORD-Eintrag
ord-38581de9b1114be4935b945dafac826a
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04035437

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