反応 #172518

ord-400216d8afdc48fb9c19b4eb29c6ea0b

溶媒

反応条件

温度
65°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The tar-like matter was separated by decantation
  2. 2
    その他purified by silica gel column chromatography
  3. 3
    その他crystallized in methanol
  4. 4
    その他separated by filtration

実験手順

In 8 ml of ethanol were dissolved 155 mg (0.33 mmol) of 5-[2-[2-benzyloxy-4-[butyl(4-hydroxybutyl)amino]phenyl]vinyl]thiophene-2-carboaldehyde and 116 mg (0.37 mmol) of 2-(3-cyano-4-methyl-5-phenyl-5-trifluoromethyl-2(5H)-furanylidene]propanedinitrile. The mixture was stirred with heating at 65° C. for 1 hour. The tar-like matter was separated by decantation, purified by silica gel column chromatography, crystallized in methanol, and separated by filtration to give 153 mg of a dark brown crystal having amp of 181-183° C. (yield: 60.2%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846955B2uspto-grants-2014_09