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Water → Piperazine, 1-[1-(4-fluorophenyl)-2-(1-piperazinyl)ethyl]-4-methyl-

HRID 497323
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HRID 497323 반응식
C(OC([N:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH:13]([C:21]2[CH:26]=[CH:25][C:24]([F:27])=[CH:23][CH:22]=2)[N:14]2[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]2)[CH2:8][CH2:7]1)=O)C.[OH-].[K+].O>C(O)C>[F:27][C:24]1[CH:25]=[CH:26][C:21]([CH:13]([N:14]2[CH2:19][CH2:18][N:17]([CH3:20])[CH2:16][CH2:15]2)[CH2:12][N:9]2[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]2)=[CH:22][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 11731626HCID 11731626, 화합물

생성물 1

HCID 10957750Piperazine, 1-[1-(4-fluorophenyl)-2-(1-piperazinyl)ethyl]-4-methyl-수율 98.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.25 g of 1-Ethoxycarbonyl-4-[2-(4-fluorophenyl)-2-(4-methylpiperazino)ethyl]piperazine was dissolved in 2 ml of ethanol, and 1.3 g of potassium hydroxide was added, followed by reflux with heating for an hour. The reaction solution was cooled to room temperature and, after addition of 2 ml of water, extracted with ethyl acetate, and the organic layer was dried over anhydrous sodium sulfate. After removal of the drying agent by filtration, the filtrate was concentrated under reduced pressure to give 1.0 g of a crude 1-[2-(4-fluorophenyl)-2-(4-methyl-piperazino)ethyl]piperazine.

후처리

  1. temperatureby reflux
  2. temperaturewith heating for an hour
  3. extractionextracted with ethyl acetate
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. customAfter removal of the drying agent
  6. filtrationby filtration
  7. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6b841a51dc914169ba715046dfc763ee
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06949552B2

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