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

HRID 49748
ノート
印刷プレビュー

反応式

HRID 49748 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 1049Pyridine
溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
8.5 °C

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%.

後処理

  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

出典と根拠

ORDレコード
ord-7025cbae4e164e20a9fa5ffa430be656
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06709804B2

反応ノート

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