تفاعل #73202

ord-2d9f4bce387e4d24b6d32858c7a0a670

المذيبات

ظروف التفاعل

درجة الحرارة
125°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe product was extracted with three portions of MTBE
  2. 2
    تجفيفThe combined extracts were dried over sodium sulfate
  3. 3
    ترشيحfiltered
  4. 4
    تركيزconcentrated

الإجراء التجريبي

A mixture of 3-methyl-3-[4-(1-[2-(trimethylsilyl)ethoxy]methyl-1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]butyl methanesulfonate (42 mg, 0.000088 mol) and potassium cyanide (46 mg, 0.000702 mol) in DMF (1 mL) was heated in the microwave reactor for 30 min at 125° C. followed by additional 30 min at 135° C. The mixture was then diluted with water, and the product was extracted with three portions of MTBE. The combined extracts were dried over sodium sulfate, filtered and concentrated to give 61 mg of crude 4-methyl-4-[4-(1-[2-(trimethylsilyl)ethoxy]methyl-1H-pyrrolo-[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]pentanenitrile, which was used without further purification. MS(ES): 410 (M+1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541425B2uspto-grants-2013_09