Isobutylene → HCID 23330246, Verbindung

HRID 224759Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 224759
[CH3:1][C:2](=[CH2:4])[CH3:3].[Cl:5][C:6]([Cl:13])([Cl:12])[CH2:7][CH2:8][C:9](Cl)=[O:10].C(N(CC)CC)C>C1CCCCC1>[Cl:5][C:6]([Cl:13])([Cl:12])[CH2:7][CH:8]1[C:2]([CH3:4])([CH3:3])[CH2:1][C:9]1=[O:10]

Komponenten

5

Edukt 3

HCID 8255IsobutyleneHCID 8471TriethylamineHCID 545309984,4,4-Trichlorobutanoyl chloride

Produkt 1

HCID 23330246HCID 23330246, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8078CyclohexaneLösungsmittel2×

Versuchsvorschrift

261 g of isobutylene is injected into a 1 liter autoclave containing 49 g (0.23 mol) of 4,4,4-trichlorobutyric acid chloride in 280 ml of cyclohexane. A solution of 28.3 g (0.28 mol) of triethylamine in 233 ml of cyclohexane is pumped in at 70° C. in the course of 4 hours. The reaction mixture is afterwards held at 70° C. for a further 4 hours. The precipitated hydrochloride of the triethylamine is filtered off; the filtrate obtained is washed with dilute hydrochloric acid and then with water, dried over sodium sulphate and concentration by evaporation. Distillation of the residue yields 2-(2',2',2'-trichloroethyl)-3,3-dimethylcyclobutanone as a clear liquid, b.p. 118°-122° C./14 mm Hg.

Aufarbeitung

  1. customis pumped in at 70° C. in the course of 4 hours
  2. filtrationThe precipitated hydrochloride of the triethylamine is filtered off
  3. customthe filtrate obtained
  4. washis washed with dilute hydrochloric acid
  5. dry with materialwith water, dried over sodium sulphate and concentration by evaporation
  6. distillationDistillation of the residue

Quellen und Nachweise

ORD-Eintrag
ord-77b2b95aaede44cab24a6058d1da66d5
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04234517

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