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Methanol → 2-Bromo-1-(1-methylcyclohexyl)ethan-1-one

HRID 1579122
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1579122
[Br:1]Br.C(Cl)(Cl)Cl.[CH3:7][C:8]([C:10]1([CH3:16])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)=[O:9].CO>BrBr.O>[CH3:16][C:10]1([C:8]([CH2:7][Br:1])=[O:9])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 887MethanolHCID 6212ChloroformHCID 24408Bromine2×HCID 5441981-(1-methylcyclohexyl)ethanone

Produkt 1

HCID 214750112-Bromo-1-(1-methylcyclohexyl)ethan-1-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24408BromineKatalysator
HCID 962
Water
Lösungsmittel

Versuchsvorschrift

A solution of 328 g. bromine in 300 ml. chloroform was added gradually to a stirred solution of 300 g. 1-methylcyclohexyl methyl ketone in 100 ml. methanol. After the addition of a few drops of bromine solution at 15°C. the reaction mixture was cooled and maintained between 0°-5°C. The reaction mixture was stirred for 10 minutes, after the addition of bromine had been completed, and then poured on to a mixture of crushed ice and water. The water layer was separated from the organic liquid and extracted with methylene chloride. The extract and the organic portion were combined and washed with water followed by a saturated solution of sodium bicarbonate and then finally with water. After drying over calcium chloride the liquid was evaporated and distilled to give bromomethyl 1-methylcyclohexyl ketone, b.p. 76°-78°C./0.1 mm.Hg.

Aufarbeitung

  1. temperaturewas cooled
  2. temperaturemaintained between 0°-5°C
  3. customThe water layer was separated from the organic liquid
  4. extractionextracted with methylene chloride
  5. extractionThe extract
  6. washwashed with water
  7. dry with materialAfter drying over calcium chloride the liquid
  8. customwas evaporated
  9. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-32b930b73ba54c8aa33d8552a0db21f5
Quelldatensatz
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03940484

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