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Hydrochloric Acid → 3,3'-Dinitro-4,4'-di-2-furoylaminobiphenyl

HRID 1859386
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인쇄 미리보기

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HRID 1859386 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[C:13]([N+:18]([O-:20])=[O:19])[CH:12]=2)[CH:7]=[CH:8][C:9]=1[NH2:10])([O-:3])=[O:2].[O:21]1[CH:25]=[CH:24][CH:23]=[C:22]1[C:26](Cl)=[O:27].Cl>O.N1C=CC=CC=1.CN(C)C=O>[N+:1]([C:4]1[CH:5]=[C:6]([C:11]2[CH:16]=[CH:15][C:14]([NH:17][C:26]([C:22]3[O:21][CH:25]=[CH:24][CH:23]=3)=[O:27])=[C:13]([N+:18]([O-:20])=[O:19])[CH:12]=2)[CH:7]=[CH:8][C:9]=1[NH:10][C:26]([C:22]1[O:21][CH:25]=[CH:24][CH:23]=1)=[O:27])([O-:3])=[O:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 682422-Furancarbonyl chlorideHCID 31067203,3'-Dinitrobenzidine

생성물 1

HCID 227415993,3'-Dinitro-4,4'-di-2-furoylaminobiphenyl수율 81.2%

시약·촉매·용매 3

HCID 962Water용매2회HCID 1049
Pyridine
용매
HCID 6228Dimethylformamide용매

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온도
8.5 °C

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-furoylaminobiphenyl. The yield was 81%.

후처리

  1. customIn a 500 ml separable flask equipped with a stirrer, a reflux condenser
  2. additionAfter the addition
  3. temperaturethe reaction solution was warmed to the room temperature
  4. customthe solid substance was separated by filtration
  5. washThe obtained solid substance was washed well with water
  6. customdried in a reduced pressure

출처 및 근거

ORD 기록
ord-1d42b8032ca049b2b8d4d562d9b369af
출처 데이터셋
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06528231B1

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