Methanesulfonic Acid → 1,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate

HRID 49295Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 49295
[CH3:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]=[CH:11][C:12]([N:15]3[CH2:21][CH2:20][CH2:19][N:18]([C:22]4[CH:27]=[CH:26][C:25]([C:28]5[CH:33]=[C:32]([CH3:34])[CH:31]=[C:30]([CH3:35])[CH:29]=5)=[CH:24][N:23]=4)[CH2:17][CH2:16]3)=[N:13][CH:14]=2)[CH:5]=[C:6]([CH3:8])[CH:7]=1.[CH3:36][S:37]([OH:40])(=[O:39])=[O:38]>CO>[CH3:36][S:37]([OH:40])(=[O:39])=[O:38].[CH3:36][S:37]([OH:40])(=[O:39])=[O:38].[CH3:8][C:6]1[CH:5]=[C:4]([C:9]2[CH:10]=[CH:11][C:12]([N:15]3[CH2:21][CH2:20][CH2:19][N:18]([C:22]4[CH:27]=[CH:26][C:25]([C:28]5[CH:33]=[C:32]([CH3:34])[CH:31]=[C:30]([CH3:35])[CH:29]=5)=[CH:24][N:23]=4)[CH2:17][CH2:16]3)=[N:13][CH:14]=2)[CH:3]=[C:2]([CH3:1])[CH:7]=1

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 206349591,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine

Produkt 1

HCID 206349601,4-Bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonateAusbeute 90,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 1,4-bis[5-(3,5-dimethylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (83.0 mg, 0.170 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.37 mL, 0.37 mmol), and the mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from ethanol-diethyl ether-hexane to yield the title compound as colorless needles [melting point: 188.0° C. (decomposed)](101.0 mg, yield: 86%).

Aufarbeitung

  1. concentrationthe mixture was concentrated under reduced pressure
  2. additionEthanol (5.0 mL) was added to the residue
  3. concentrationthe resulting mixture was concentrated under reduced pressure
  4. customThe residue was recrystallized from ethanol-diethyl ether-hexane

Quellen und Nachweise

ORD-Eintrag
ord-c371c5b1a1fe4433a20455a57571acb6
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06706703B2

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