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Sodium Hydroxide → 3-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate

HRID 1274076
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1274076
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9](Cl)[CH2:10][C:4]=2[CH:3]=1.Cl.Cl.[CH3:20][N:21]1[CH:26]2[CH2:27][CH2:28][CH:22]1[CH2:23][NH:24][CH2:25]2.[C:29](=[O:32])([OH:31])[O-].[Na+].[OH-:34].[Na+]>CCOCC.CN(C)C=O>[C:5]([OH:34])(=[O:6])/[CH:4]=[CH:10]\[C:29]([OH:31])=[O:32].[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9]([N:24]3[CH2:25][CH:26]4[N:21]([CH3:20])[CH:22]([CH2:28][CH2:27]4)[CH2:23]3)[CH2:10][C:4]=2[CH:3]=1
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Komponenten

7

Edukt 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 221201882,10-Dichloro-10,11-dihydro-dibenz[b,f]oxepinHCID 221201898-Methyl-3,8-diazabicyclo(3.2.1)octane dihydrochloride

Produkt 1

HCID 867545003-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate

Reagenzien, Katalysatoren, Lösungsmittel

2
HCID 3283Diethyl EtherLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 2,10-Dichloro-10,11-dihydro-dibenz[b,f]oxepin (3.2 g), 8-Methyl-3,8-diazabicyclo(3.2.1)octane dihydrochloride (1.6 g), sodium bicarbonate (10 g), and dimethylformamide (40 mL) was stirred at 100° C. for 1 h. After cooling, the reaction mixture was poured onto water, made basic with NaOH and the products are extracted with ether. The ether layer was extracted with 3N HCl, the aqueous layer is basified and the basic product was reextracted with ether. After drying over magnesium sulfate the solvent was removed in vacua. The residue is dissolved in ethanol and 500 mg of maleic acid was added and the mixture was warmed until a clear solution is obtained. After dilution of this mixture with ether and cooling at -20° C. overnight, 3-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate (Compound 1) melting at 169-170° C. was obtained as white crystals.

Aufarbeitung

  1. temperatureAfter cooling
  2. additionthe reaction mixture was poured onto water
  3. extractionthe products are extracted with ether
  4. extractionThe ether layer was extracted with 3N HCl
  5. dry with materialAfter drying over magnesium sulfate the solvent
  6. customwas removed in vacua
  7. dissolutionThe residue is dissolved in ethanol
  8. addition500 mg of maleic acid was added
  9. temperaturethe mixture was warmed until a clear solution
  10. customis obtained

Quellen und Nachweise

ORD-Eintrag
ord-8172bec9b053490fbec03d37e81ed877
Quelldatensatz
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06156751

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