反応 #1095870

ord-05a15af1c2944caf9098e14e05eaabb9

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度The reaction mixture was cooled to near room temperature
  3. 3
    洗浄the mixture was washed with a saturated sodium chloride aqueous solution three times
  4. 4
    乾燥The organic layers were dried over anhydrous magnesium sulfate
  5. 5
    濃縮concentrated

実験手順

Into 2 ml of N,N-dimethylformamide was resolved 183 mg of 4-chloro-6-(2-butynyloxy)pyrimidine, 166 mg of potassium carbonate and 85 mg of 2-methylpyrrolidine was added therein, and the mixture was stirred for 7 hours at 60° C. The reaction mixture was cooled to near room temperature, ethyl acetate was added therein, and the mixture was washed with a saturated sodium chloride aqueous solution three times. The organic layers were dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 207 mg of 4-(2-butynyloxy)-6-(2-methyl-pyrrolidin-1-yl)pyrimidine (hereinafter, referred to as Compound (21)).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07973028B2uspto-grants-2011_07