反応 #72691

ord-90ce4c8ad50f4e4aa7af55ff18e28333

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度Following cooling to room temperature
  2. 2
    濃縮concentration under reduced pressure
  3. 3
    その他the residue was purified by flash chromatography (silica; 3% methanol in dichloromethane)

実験手順

A solution of 4-chloropyrrolo[2,3-d]pyrimidine (2.4 grams, 15.9 mmol), prepared by the method of Davoll, J. Am. Chem. Soc., 82, 131 (1960), which is incorporated by reference in its entirety, and the product from Method A (1.7 grams, 7.95 mmol) dissolved in 2 equivalents of triethylamine was heated in a sealed tube at 100° C. for 3 days. Following cooling to room temperature and concentration under reduced pressure, the residue was purified by flash chromatography (silica; 3% methanol in dichloromethane) affording 1.3 grams (50%) of the title compound as a colorless oil. LRMS: 336.1 (M+1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541426B2uspto-grants-2013_09