反応 #1492201

ord-fd82339a7072408c8a8ca16cd016e610

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮For the work-up the reaction mixture is concentrated in vacuo before water
  2. 2
    workup.ADDITIONis added
  3. 3
    その他The precipitate is collected
  4. 4
    その他dried at 40° C.
  5. 5
    その他crystallized from MeOH/H2O

実験手順

The title compound is synthesized according to general procedure GP2 starting from 4.0 g (15 mmol) 4-chloro-5-iodo-6-methyl-pyrimidin-2-ylamine (GP3) and 2.0 g (19 mmol) 3-ethynyl-pyridine using 282 mg (1.5 mmol) CuI, 1.0 g (1.5 mmol) PdCl2(PPh3)2 and 21 mL (148 mmol) triethylamine in 200 mL dry DMF. For the work-up the reaction mixture is concentrated in vacuo before water is added. The precipitate is collected, dried at 40° C. and crystallized from MeOH/H2O. Yield: 3.0 g (83%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08916548B2uspto-grants-2014_12