Vinylidene chloride → 1,1-Dichloro-3,3,4-trimethylpent-1-ene

HRID 1253130Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1253130
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]([Cl:8])([Cl:7])=[CH2:6].Cl[C:10]([CH3:15])([CH:12]([CH3:14])[CH3:13])[CH3:11]>C(O)(=O)C>[Cl:7][C:5]([Cl:8])=[CH:6][C:10]([CH3:15])([CH3:11])[CH:12]([CH3:14])[CH3:13]

Komponenten

5

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

20 g of anhydrous, powdered aluminum chloride are added in portions to 2,040 g (21 mols) of vinylidene chloride at -10° C., in a dry apparatus equipped with a drying tube. 837 g (7 mols) of 2-chloro-2,3-dimethylbutane are then added dropwise in the temperature range from 0° to 10° C. The mixture is allowed to warm up to 20° C., and further aluminum chloride portions (a maximum of 20 g) are added, while cooling, until the reaction is no longer exothermic. The mixture is stirred for a further 4 hours at room temperature, the catalyst is deactivated by dropwise addition of 70 ml of acetic acid, and the mixture is filtered over sodium sulphate. The volatile constituents are separated from the sparingly volatile constituents by continuous-feed distillation under 1 mbar. The distillate is fractionated in a column. 824 g (65% of theory) of 1,1-dichloro-3,3,4-trimethyl-pent-1-ene of boiling point 60°-75° C./20 mbar are obtained. ##STR19##

Aufarbeitung

  1. customequipped with a drying tube
  2. temperaturewhile cooling, until the reaction
  3. filtrationthe mixture is filtered over sodium sulphate
  4. customThe volatile constituents are separated from the sparingly volatile constituents by continuous-feed distillation under 1 mbar

Quellen und Nachweise

ORD-Eintrag
ord-863c4439291d4ced802e61be3e1e32d8
Quelldatensatz
uspto-grants-1988_05
Patentnummer
US04747869

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