تفاعل #164523

ord-e1d09784d5e745e89ef2dfc6d17429fa

المذيبات

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter the addition, reaction mixture
  2. 2
    درجة الحرارةmaintained for 30 hrs
  3. 3
    درجة الحرارةThe reaction mixture was cooled to room temperature 28° C.
  4. 4
    ترشيحfiltered
  5. 5
    workup.DISTILLATIONThe solvent was distilled off
  6. 6
    أخرىto get the product

الإجراء التجريبي

To 37.63 gm (0.3163 mole) of benzotriazole and 35 gm of potassium carbonate in Dimethylformamide (DMF) (350 ml) was added slowly under stirring 82 gm of 2-chloromethyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane (intermediate for compound 7) in DMF (300 ml). After the addition, reaction mixture was heated to 120° C. and maintained for 30 hrs. The reaction mixture was cooled to room temperature 28° C. and filtered. The solvent was distilled off to get the product. It was a thick dark brown liquid. Yield of product was 90%

المصدر

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