Dichloromethane → 1-bromo-2-chloro-4-ethynylbenzene

HRID 1018810Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1018810
[OH-].[Na+].Cl[C:4]([C:8]1[CH:13]=[CH:12][C:11]([Br:14])=[C:10]([Cl:15])[CH:9]=1)=[CH:5]C=O.ClCCl>O.O1CCOCC1>[Br:14][C:11]1[CH:12]=[CH:13][C:8]([C:4]#[CH:5])=[CH:9][C:10]=1[Cl:15]

Komponenten

6

Edukt 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 57087279HCID 57087279, Verbindung

Produkt 1

HCID 223904241-bromo-2-chloro-4-ethynylbenzene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 312751,4-DioxaneLösungsmittel2×

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

40 g of sodium hydroxide are dissolved, under an inert atmosphere, in 230 ml of water, 120 ml of 1,4-dioxane are added and the reaction mixture is heated to 80° C. 17.5 g of 3-chloro-3-(4-bromo-3-chlorophenyl)propenal dissolved in 400 ml of 1,4-dioxane are added and the reaction mixture is stirred for 30 minutes at 80° C. The reaction mixture is allowed to cool to room temperature and 2300 ml of dichloromethane are then added. The phases are separated after settling has taken place and the organic phase is washed with water and dried over magnesium sulphate. The compound dissolved in a dichloromethane/1,4-dioxane mixture is used in its current form in the next step.

Aufarbeitung

  1. additionare added
  2. temperatureto cool to room temperature
  3. customThe phases are separated after settling
  4. washthe organic phase is washed with water
  5. dry with materialdried over magnesium sulphate
  6. dissolutionThe compound dissolved in a dichloromethane/1,4-dioxane mixture

Quellen und Nachweise

ORD-Eintrag
ord-e9067f02cceb403792f678d8f0261533
Quelldatensatz
uspto-grants-2002_11
Patentnummer
US06482986B1

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