Benzenesulfonic Acid → HCID 11670737, Verbindung

HRID 604830Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 604830
[CH:1]1([CH2:4][N:5]2[CH2:10][CH2:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:17]3[CH2:22][C:21]([CH3:24])([CH3:23])[CH2:20][C:19]([CH3:26])([CH3:25])[CH2:18]3)[CH2:7][CH2:6]2)[CH2:3][CH2:2]1.[C:27]1([S:33]([OH:36])(=[O:35])=[O:34])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>CO>[C:27]1([S:33]([OH:36])(=[O:35])=[O:34])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.[CH:1]1([CH2:4][N:5]2[CH2:6][CH2:7][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[CH:17]3[CH2:18][C:19]([CH3:26])([CH3:25])[CH2:20][C:21]([CH3:24])([CH3:23])[CH2:22]3)[CH2:9][CH2:10]2)[CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 7371Benzenesulfonic AcidHCID 11302685Piperazine, 1-(cyclopropylmethyl)-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]-

Produkt 1

HCID 11670737HCID 11670737, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To 1-cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (300 mg, 0.846 mmol) were added methyl alcohol (2.5 mL) and benzenesulfonic acid (136 mg, 0.863 mmol) to form a thoroughly dissolved state, followed by concentration under reduced pressure. To the obtained residual oil was added ethyl acetate to dissolve, and the mixture was allowed to stand. The suspension containing precipitated crystals was concentrated to dryness under reduced pressure. Diethyl ether was added thereto, and the solid was triturated by sonication. Precipitated crystals were collected by filtration, washed with diethyl ether, and aircured by aspiration. Drying under reduced pressure using a vacuum pump at room temperature gave 425 mg of the title compound as colorless crystals.

Aufarbeitung

  1. customto form a thoroughly dissolved state
  2. concentrationfollowed by concentration under reduced pressure
  3. additionTo the obtained residual oil was added ethyl acetate
  4. dissolutionto dissolve
  5. additionThe suspension containing
  6. customprecipitated crystals
  7. concentrationwas concentrated to dryness under reduced pressure
  8. additionDiethyl ether was added
  9. customthe solid was triturated by sonication
  10. customPrecipitated crystals
  11. filtrationwere collected by filtration
  12. washwashed with diethyl ether
  13. customDrying under reduced pressure
  14. customat room temperature

Quellen und Nachweise

ORD-Eintrag
ord-8aa4fe1b1e0843f6ae84c13eb4241c61
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07910734B2

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