Ethyl Acetate → Cutamesine

HRID 1014952Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1014952
Cl.Cl.[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH2:13][CH2:14][N:15]2[CH2:20][CH2:19][N:18]([CH2:21][CH2:22][CH2:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:17][CH2:16]2)[CH:8]=[CH:9][C:10]=1[O:11][CH3:12].[OH-].[Na+].C(OCC)(=O)C>C1COCC1.[Cl-].[Na+].O>[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH2:13][CH2:14][N:15]2[CH2:16][CH2:17][N:18]([CH2:21][CH2:22][CH2:23][C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:19][CH2:20]2)[CH:8]=[CH:9][C:10]=1[O:11][CH3:12]

Komponenten

6

Edukt 3

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 9954941SA 4503

Produkt 1

HCID 9907323CutamesineAusbeute 93,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

To a suspension of 1-[2-(3,4-dimethoxyphenyl)ethyl]-4-(3-phenylpropyl)piperazine dihydrochloride (1.06 g, 2.40 mmol) in THF (5 mL) is added a solution of sodium hydroxide (1N, 6 mL). To the resulting solution is added ethyl acetate and brine. The organic layer is separated, filtered through silica gel, dried over anhydrous sodium sulfate, concentrated, and dried to give 0.829 g of 1-[2-(3,4-dimethoxyphenyl)ethyl]-4-(3-phenylpropyl)piperazine as a light brown solid.

Aufarbeitung

  1. customThe organic layer is separated
  2. filtrationfiltered through silica gel
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-722923559f4c4364a9b5be0e338215c9
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07985751B2

Notizen zur Reaktion

Wird geladen…