Water → HCID 22273264、化合物

HRID 1064357ノート

反応式

HRID 1064357 の反応式
[Cl:1][C:2]1[C:8](Cl)=[CH:7][C:5]([NH2:6])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.[NH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.C(=O)([O-])[O-].[Na+].[Na+].O>C1(O)CCCCC1>[Cl:1][C:2]1[C:8]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[CH:7][C:5]([NH2:6])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 4837PiperazineHCID 10340Sodium CarbonateHCID 811494,5-Dichloro-2-nitroaniline

生成物 1

HCID 22273264HCID 22273264、化合物収率 84.9%

試薬・触媒・溶媒 1

HCID 7966Cyclohexanol溶媒

反応条件

温度
150 °C

実験手順

Into a solution of 20.02 g of 4,5-dichloro-2-nitroaniline and 8.70 g of piperazine in 100 ml of cyclohexanol, 12.80 g of sodium carbonate was added and stirred at 150° C. for 14 hours. Cooling the reaction liquid to room temperature, water was added and the system was extracted with chloroform. The chloroform layer was dried on anhydrous magnesium sulfate and the solvent was distilled off. Thus obtained residue was washed with diisopropyl ether to provide 21.07 g of 4-chloro-2-nitro-5-(piperazin-1-yl) aniline as a yellow powder.

後処理

  1. temperatureCooling
  2. customthe reaction liquid to room temperature
  3. extractionthe system was extracted with chloroform
  4. dry with materialThe chloroform layer was dried on anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off
  6. washThus obtained residue was washed with diisopropyl ether

出典と根拠

ORDレコード
ord-bc7791d27df84f43bfad8bc268e4517b
出典データセット
uspto-grants-2005_11
特許番号
US06969712B2

反応ノート

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