Reaktion #164520

Reaktionsgleichung

2-chloro-5-chloromethylthiazole

sodium hydride

2-hydroxymethyl-8-phenethyl-1,4-dioxa-8-azaspiro[4,5]decane

→

2-(2-chloro-5-thiazolyl)methoxymethyl-8-phenethyl-1,4-dioxa-8-azaspiro[4,5]decane

Lösungsmittel

toluene

toluene

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction mixture was refluxed for 15 hrs
2. 2
   WaschenThe reaction mixture was washed with water
3. 3
   Extraktionthe product was extracted with methylene chloride 100 ml
4. 4
   workup.DISTILLATIONThe solvent was distilled off
5. 5
   Sonstigeto get thick dark colored liquid

Vorschrift

To 8.64 g (0.36 mole) of sodium hydride in toluene (250 ml) was added 2-hydroxymethyl-8-phenethyl-1,4-dioxa-8-azaspiro[4,5]decane (compound 1.50 gm, 0.18 mole) in toluene (350 ml) with stirring at 28° C. The phase transfer catalyst tetrabutylammonium bromide TBAB 2 gm was added and 31 gm of 2-chloro-5-chloromethylthiazole in toluene (225 ml) was then added drop wise at 10° C. and the reaction mixture was refluxed for 15 hrs. The reaction mixture was washed with water and the product was extracted with methylene chloride 100 ml. The solvent was distilled off to get thick dark colored liquid. The yield of the product was 85%.

Quelle