反応 #69168

ord-e19397aff2784f2fadad6fd74058fa94

溶媒

反応条件

温度
125°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the product was extracted with three portions of MTBE
  2. 2
    乾燥The combined extracts were dried over sodium sulfate
  3. 3
    ろ過filtered
  4. 4
    濃縮concentrated

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530485B2uspto-grants-2013_09