反応 #78026

ord-7025cbae4e164e20a9fa5ffa430be656

反応条件

温度
8.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他In a 500 ml separable flask equipped with a stirrer, a reflux condenser
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    温度the reaction solution was warmed to the room temperature
  4. 4
    その他the solid substance was separated by filtration
  5. 5
    洗浄The obtained solid substance was washed well with water
  6. 6
    その他dried in a reduced pressure

実験手順

In a 500 ml separable flask equipped with a stirrer, a reflux condenser cooled with water, a thermometer and a dropping funnel, 10.96 g of 3,3′-dinitro-4,4′-diaminobiphenyl was dissolved into 200 ml of N,N-dimethylformamide and then 20 ml of pyridine was added to the solution. While the prepared solution was cooled at 3 to 14° C., 12.53 g of 2-furoyl chloride was added dropwise to the solution. After the addition was completed, the reaction solution was warmed to the room temperature and stirred for further 5 hours. Then, 80 ml of 2N hydrochloric acid and 100 ml of water were added to the solution and the solid substance was separated by filtration. The obtained solid substance was washed well with water and dried in a reduced pressure to obtain 15.0 g of 3,3′-dinitro-4,4′-di-2-furoylamino-biphenyl. The yield was 81%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06709804B2uspto-grants-2004_03