Water → HCID 22273264, 화합물

HRID 1064357노트

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HRID 1064357 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 22273264HCID 22273264, 화합물수율 84.9%

시약·촉매·용매 1

HCID 7966Cyclohexanol용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bc7791d27df84f43bfad8bc268e4517b
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969712B2

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