반응 #73202

ord-2d9f4bce387e4d24b6d32858c7a0a670

용매

반응 조건

온도
125°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the product was extracted with three portions of MTBE
  2. 2
    건조The combined extracts were dried over sodium sulfate
  3. 3
    여과filtered
  4. 4
    농축concentrated

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541425B2uspto-grants-2013_09