1-Ethylpiperazine → 1-[2-Hydroxy-3-(4-ethyl-1-piperazinyl)-4-oxo-2-cyclobuten-1-ylidene]-4-ethylpiperazinium hydroxide

HRID 2072285Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2072285
[NH:1]([C:8]1[C:9](=[O:20])[C:10](=[N:13][C:14]2[CH:19]=CC=CC=2)[C:11]=1[OH:12])[C:2]1[CH:7]=CC=CC=1.C(N1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1)C>>[OH-:12].[OH:12][C:11]1[C:10](=[N+:13]2[CH2:14][CH2:19][N:26]([CH2:25][CH3:24])[CH2:27][CH2:28]2)[C:9](=[O:20])[C:8]=1[N:1]1[CH2:2][CH2:7][N:1]([CH2:8][CH3:11])[CH2:2][CH2:7]1

Komponenten

3

Edukt 2

HCID 791961-EthylpiperazineHCID 109783293-Hydroxy-2-(phenylamino)-4-(phenylimino)-2-cyclobuten-1-one

Produkt 1

HCID 214077921-[2-Hydroxy-3-(4-ethyl-1-piperazinyl)-4-oxo-2-cyclobuten-1-ylidene]-4-ethylpiperazinium hydroxide

Versuchsvorschrift

A mixture of 4.0 grams of 2-anilino-3-hydroxy-4-(phenylimino)-2-cyclobuten-1-one and 3.4 grams of 1-ethylpiperazine is heated at 194°-198° C. in an atmosphere of dry nitrogen for 30 minutes. The cooled solid is comminuted, washed with anhydrous ethyl ether, and dried and the resulting solid is then extracted with 50 ml. of anhydrous benzene. The benzene solution is treated with activated carbon, filtered, concentrated and cooled. A crystalline solid forms and this is separated by filtration and dissolved in distilled water at room temperature and the solution is filtered and concentrated. A precipitate forms and is separated by filtration to give 1-[2-hydroxy-3-(4-ethyl-1-piperazinyl)-4-oxo-2-cyclobuten-1-ylidene]-4-ethylpiperazinium hydroxide inner salt melting at about 179.5°-183° C.

Aufarbeitung

  1. temperatureis heated at 194°-198° C. in an atmosphere of dry nitrogen for 30 minutes
  2. customThe cooled solid is comminuted
  3. washwashed with anhydrous ethyl ether
  4. customdried
  5. extractionthe resulting solid is then extracted with 50 ml
  6. additionThe benzene solution is treated with activated carbon
  7. filtrationfiltered
  8. concentrationconcentrated
  9. temperaturecooled
  10. customA crystalline solid forms and this is separated by filtration
  11. dissolutiondissolved in distilled water at room temperature
  12. filtrationthe solution is filtered
  13. concentrationconcentrated
  14. customA precipitate forms and is separated by filtration

Quellen und Nachweise

ORD-Eintrag
ord-bcf2d8722c2044219b712fbdd28e19d7
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04051136

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