反応 #40364

ord-7ccb126b89ca40838648d5c99efc243b

反応条件

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 refluxed for 20 hrs
  3. 3
    濃縮The reaction mixture was concentrated in vacuo
  4. 4
    workup.ADDITIONdiluted with ethyl acetate
  5. 5
    洗浄washed with water
  6. 6
    乾燥The organic layer was dried over magnesium sulfate
  7. 7
    濃縮concentrated in vacuo
  8. 8
    その他yielded 220 mg (59%) with a purity of 72% log P (pH=2.3)=1.45

実験手順

To a mixture of 310 mg (0.8 mmol) of 4-[(2-chloro-6-methylpyrimidin-4-yl)oxy]-2,5-dimethyl-aniline in 20 ml acetonitrile 208 mg (1.5 mmol) of N-(dimethoxymethyl)-N-methylethanamine (77% pure) was added. The reaction mixture was refluxed for 20 hrs. The reaction mixture was concentrated in vacuo, diluted with ethyl acetate and washed with water. The organic layer was dried over magnesium sulfate and concentrated in vacuo yielded 220 mg (59%) with a purity of 72% log P (pH=2.3)=1.45.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07727986B2uspto-grants-2010_06