反応 #1704435

ord-ad4ec7d8ce0644ba867c6d46e99c837c

反応条件

温度
155°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling the mixture
  2. 2
    ろ過The precipitate was filtered
  3. 3
    洗浄washed with water
  4. 4
    乾燥50% EtOH/ether and dried

実験手順

A stirred mixture of (4-mercaptophenyl)methanol (6.72 g), 2-amino-5-bromo-6-methylpyrimidin-4-ol (10.76 g) and K2 CO3 (7.29 g) in ethylene glycol (120 ml) was heated at 155° C. for 9 h. After cooling the mixture was poured into water (500 ml) and neutralised with conc. HCl. The precipitate was filtered, washed with water then 50% EtOH/ether and dried to give the subtitle compound as a solid, 6.7 g. 1H NMR DMSO-d6: δ11.07 (brs, 1H); 7.18 (d, 2H); 6.99 (d, 2H); 6.87 (brs, 2H); 5.09 (s, 1H); 4.41 (s, 2H); 2.24 (s, 3H)

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08765939B2uspto-grants-2014_07