Water → 2-Chloromethyl-5,5-dimethyl-2-(2,5-dimethylphenyl)-[1,3]dioxane

HRID 1866787Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1866787
[Cl:1][CH2:2][C:3]([C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:6]=1[CH3:12])=[O:4].[CH3:13][C:14]([CH3:19])([CH2:17]O)[CH2:15][OH:16].O>C1(C)C(C)=CC=CC=1>[Cl:1][CH2:2][C:3]1([C:5]2[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:6]=2[CH3:12])[O:16][CH2:15][C:14]([CH3:19])([CH3:17])[CH2:13][O:4]1

Komponenten

5

Edukt 3

HCID 962Water2×HCID 31344Neopentyl glycolHCID 23636932-Chloro-1-(2,5-dimethylphenyl)ethan-1-one

Produkt 1

HCID 578106312-Chloromethyl-5,5-dimethyl-2-(2,5-dimethylphenyl)-[1,3]dioxane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel2×

Versuchsvorschrift

0.5 mol of 2-chloro-1-(2,5-dimethylphenyl)ethanone, 104 g [1 mol] of 2,2-dimethyl-1,3-propanediol (neopentyl glycol) and 9.5 g [0.05 mol] of p-TsOH hydrate are boiled in 500 ml of xylene with a water trap until the formation of water ceases (about 4 hours). 200 ml of water and 30 ml of xylene are added to the reaction mixture at room temperature. A better phase separation is achieved by adding 50 ml of saturated aqueous NaCl solution. The organic phase is then extracted again with 100 ml of water and 100 ml of saturated aqueous NaCl solution, dried and concentrated.

Aufarbeitung

  1. customA better phase separation
  2. additionby adding 50 ml of saturated aqueous NaCl solution
  3. extractionThe organic phase is then extracted again with 100 ml of water and 100 ml of saturated aqueous NaCl solution
  4. customdried
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-80474765957f4da28dad361605b63493
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07629476B2

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