반응 #78026

ord-7025cbae4e164e20a9fa5ffa430be656

반응 조건

온도
8.5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타In a 500 ml separable flask equipped with a stirrer, a reflux condenser
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    온도the reaction solution was warmed to the room temperature
  4. 4
    기타the solid substance was separated by filtration
  5. 5
    세척The obtained solid substance was washed well with water
  6. 6
    기타dried in a reduced pressure

실험 절차

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%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06709804B2uspto-grants-2004_03