تفاعل #164520

ord-2cfa75405cf349088974236ec659b8bc

المذيبات

ظروف التفاعل

درجة الحرارة
28°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction mixture was refluxed for 15 hrs
  2. 2
    غسيلThe reaction mixture was washed with water
  3. 3
    استخلاصthe product was extracted with methylene chloride 100 ml
  4. 4
    workup.DISTILLATIONThe solvent was distilled off
  5. 5
    أخرىto get thick dark colored liquid

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08841296B2uspto-grants-2014_09