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

HRID 497323
ノート
印刷プレビュー

反応式

HRID 497323 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 11731626HCID 11731626、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6b841a51dc914169ba715046dfc763ee
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06949552B2

反応ノート

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