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Hydrochloric Acid → HCID 21183852, Verbindung

HRID 1384840
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1384840
[C:1]([C:4]1[C:5]2[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:6]=2[S:7][CH:8]=1)(=[O:3])[CH3:2].[ClH:14].[CH3:15][O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.Cl.[CH2:30]=O>CCO.C(OCC)C>[ClH:14].[ClH:14].[CH3:13][C:11]1[CH:10]=[CH:9][C:6]2[S:7][CH:8]=[C:4]([C:1](=[O:3])[CH2:2][CH2:30][N:26]3[CH2:27][CH2:28][N:23]([C:18]4[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=4[O:16][CH3:15])[CH2:24][CH2:25]3)[C:5]=2[CH:12]=1
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Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 600381HCID 600381, VerbindungHCID 9899402N-(2-Methoxyphenyl)piperazine hydrochloride

Produkt 1

HCID 21183852HCID 21183852, VerbindungAusbeute 10 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

650 mg of 3-acetyl-5-methylbenzo[b]thiophene (3.42×10−3 moles) and 860 mg of 2-methoxyphenylpiperazine hydrochloride (3.76×10−3 moles) were dissolved in 15 ml of EtOH and HCl to pH=2-3. When the mixture was under reflux, 310 mg of paraformaldehyde (10×10−3 moles) were added. After 24 hours stirring under reflux the reaction mixture was poured over ice and was extracted with AcOEt. It was washed with H2O and dried with Na2SO4, the solvent being removed to dryness. It was purified in silica column using AcOEt/hexane (1:1) as mobile phase. The oil obtained was dissolved in ethyl ether (20 ml) and EtOH (4 ml) and precipitates as hydrochloride on adding HCl(c). Yield: 10%.

Aufarbeitung

  1. temperatureunder reflux
  2. temperatureunder reflux the reaction mixture
  3. additionwas poured over ice
  4. extractionwas extracted with AcOEt
  5. washIt was washed with H2O
  6. dry with materialdried with Na2SO4
  7. customthe solvent being removed to dryness
  8. customIt was purified in silica column
  9. customThe oil obtained
  10. customEtOH (4 ml) and precipitates as hydrochloride
  11. additionon adding HCl(c)

Quellen und Nachweise

ORD-Eintrag
ord-5c5578cbc90543d1acf45c751de06abd
Quelldatensatz
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06262056B1

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