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Hydrochloric Acid → 3-[4-(3-Chlorophenyl)piperazin-1-yl]propan-1-amine

HRID 373589
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 373589
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH:18]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.CO>O>[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][NH2:18])[CH2:13][CH2:14]2)[CH:6]=[CH:7][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 19810680HCID 19810680, Verbindung

Produkt 1

HCID 35067593-[4-(3-Chlorophenyl)piperazin-1-yl]propan-1-amineAusbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Gaseous hydrochloric acid is introduced for 10 min into a round bottom flask containing 11.2 g (22.6 mmol) of 3-[4-(3-chlorophenyl]piperazin-1-yl]-N-(triphenylmethyl)propanamine and 300 ml of methanol, while the mixture is cooled in a bath of iced water. The mixture is allowed to return to room temperature and is then heated under reflux for 5.5 h. The solution is reduced to half its volume and is allowed to cool. The solid which precipitates is filtered off, is treated with water and aqueous ammonia, the mixture is extracted with ethyl acetate, the organic phase is washed with water and is dried and the solvent is evaporated off. 3.9 g of light yellow oil are obtained.

Aufarbeitung

  1. customto return to room temperature
  2. temperatureis then heated
  3. temperatureunder reflux for 5.5 h
  4. temperatureto cool
  5. customThe solid which precipitates
  6. filtrationis filtered off
  7. additionis treated with water and aqueous ammonia
  8. extractionthe mixture is extracted with ethyl acetate
  9. washthe organic phase is washed with water
  10. customis dried
  11. customthe solvent is evaporated off

Quellen und Nachweise

ORD-Eintrag
ord-847f67f3482f4ecda0dd398ff8783271
Quelldatensatz
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05164397

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