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

HRID 2072285ノート

反応式

HRID 2072285 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bcf2d8722c2044219b712fbdd28e19d7
出典データセット
uspto-grants-1977_09
特許番号
US04051136

反応ノート

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