Water → 5-(3-Carboxypiperazin-1-yl)-4-chloro-2-nitroaniline

HRID 1064359노트

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HRID 1064359 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][CH:14]1[C:19]([OH:21])=[O:20].C(=O)([O-])[O-].[Na+].[Na+].O>C1(O)CCCCC1>[C:19]([CH:14]1[NH:13][CH2:18][CH2:17][N:16]([C:8]2[C:2]([Cl:1])=[CH:3][C:4]([N+:10]([O-:12])=[O:11])=[C:5]([CH:7]=2)[NH2:6])[CH2:15]1)([OH:21])=[O:20]

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 811494,5-Dichloro-2-nitroanilineHCID 2723758Piperazine-2-carboxylic acid

생성물 1

HCID 222729645-(3-Carboxypiperazin-1-yl)-4-chloro-2-nitroaniline수율 72.1%

시약·촉매·용매 1

HCID 7966Cyclohexanol용매

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온도
150 °C

실험 절차

To a solution of 2.10 g of 4,5-dichloro-2-nitroaniline and 2.20 g of 2-piperazinecarboxylic acid in 20 ml of cyclohexanol, 4.80 g of sodium carbonate was added, followed by 14 hours' stirring at 150° C. After cooling the reaction liquid to room temperature, water was added and the system was washed with chloroform. The aqueous layer was purified with an ion-exchange resin (Diaion HP-20, Mitsubishi Kasei, eluent: methanol). Upon condensing the fraction containing the object product under reduced pressure, 2.20 g of the title compound was obtained.

후처리

  1. temperatureAfter cooling
  2. customthe reaction liquid to room temperature
  3. washthe system was washed with chloroform
  4. customThe aqueous layer was purified with an ion-exchange resin (Diaion HP-20, Mitsubishi Kasei, eluent: methanol)
  5. customUpon condensing the fraction
  6. additioncontaining the object product under reduced pressure

출처 및 근거

ORD 기록
ord-5da0a42d4ec442708176b763c252be1f
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969712B2

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