反応 #3249

ord-c39dc7ddfdaf41718ff28171b32b7253

反応条件

温度
160°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was cooled by air
  2. 2
    その他to obtain a precipitated crystal
  3. 3
    ろ過by filtration
  4. 4
    その他The crystal obtained
  5. 5
    洗浄was washed with ethanol

実験手順

A mixture of 2-amino-4-methoxybenzophenone (20 g, 88 mmol), diethylmalonate (26.7 ml, 176 mmol), 1,8-diazabicyclo[5,2,0]-undeca-7-en (DBU) (0.66 ml, 4.4 mmol) was stirred with heat at 160° C. for 2 hours. The reaction mixture was cooled by air. To the cooled mixture was added ethanol (30 ml) to obtain a precipitated crystal by filtration. The crystal obtained was washed with ethanol to give 25.7 g (yield: 90.2%) of the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05733918uspto-grants-1998_03