反応 #165580

ord-16fa0f228d654dfbbf3ae26fb3ac0464

反応条件

温度
85°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled to ambient temperature
  2. 2
    その他the resulting solid was triturated with isopropanol
  3. 3
    その他Recrystallization from hot ethanol

実験手順

A mixture of 4-methylthiazol-2-ylamine (0.75 g, 6.5 mmol) and 2-bromoethyl methyl ether (730 μL, 7.8 mmol) was heated at 85° C. for 15 hours. The mixture was cooled to ambient temperature and the resulting solid was triturated with isopropanol. Recrystallization from hot ethanol afforded 0.56 g (34%) of the title compound. 1H NMR (DMSO-d6, 300 MHz) δ ppm 2.25 (d, J=1.4 Hz, 3H) 3.25 (s, 3H) 3.57 (t, J=5.1 Hz, 2H) 4.15 (t, J=5.1 Hz, 2H) 6.68 (d, J=1.4 Hz, 1H) 9.40 (s, 1H); MS (DCI/NH3) m/z 173 (M+H)+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08841334B2uspto-grants-2014_09