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

HRID 49299Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 49299
[O:1]([C:4]1[CH:5]=[C:6]([C:16]2[CH:17]=[CH:18][C:19]([N:22]3[CH2:28][CH2:27][CH2:26][N:25]([C:29]4[CH:34]=[CH:33][C:32]([C:35]5[CH:40]=[C:39]([O:41][CH2:42][CH3:43])[C:38]([O:44][CH2:45][CH3:46])=[C:37]([O:47][CH2:48][CH3:49])[CH:36]=5)=[CH:31][N:30]=4)[CH2:24][CH2:23]3)=[N:20][CH:21]=2)[CH:7]=[C:8]([O:13][CH2:14][CH3:15])[C:9]=1[O:10][CH2:11][CH3:12])[CH2:2][CH3:3].[CH3:50][S:51]([OH:54])(=[O:53])=[O:52]>CO>[CH3:50][S:51]([OH:54])(=[O:53])=[O:52].[CH3:50][S:51]([OH:54])(=[O:53])=[O:52].[CH2:48]([O:47][C:37]1[CH:36]=[C:35]([C:32]2[CH:33]=[CH:34][C:29]([N:25]3[CH2:26][CH2:27][CH2:28][N:22]([C:19]4[CH:18]=[CH:17][C:16]([C:6]5[CH:7]=[C:8]([O:13][CH2:14][CH3:15])[C:9]([O:10][CH2:11][CH3:12])=[C:4]([O:1][CH2:2][CH3:3])[CH:5]=5)=[CH:21][N:20]=4)[CH2:23][CH2:24]3)=[N:30][CH:31]=2)[CH:40]=[C:39]([O:41][CH2:42][CH3:43])[C:38]=1[O:44][CH2:45][CH3:46])[CH3:49]

Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 206349381,4-Bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine

Produkt 1

HCID 206349391,4-Bis[5-(3,4,5-triethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonateAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 1,4-bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (77 mg, 0.115 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.23 mL, 0.23 mmol), and the reaction 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 methanol-diethyl ether to yield the title compound as a pale yellow crystalline powder (melting point: 235.0-237.0° C.) (74.0 mg, yield: 94%).

Aufarbeitung

  1. concentrationthe reaction 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 methanol-diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-837cc1f0d66546d0a7a435edf2e40bf1
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06706703B2

Notizen zur Reaktion

Wird geladen…