Dimethylformamide → 11-{1-[2-(Phenyl)ethyl]piperidin-4-yl}-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine oxalate

HRID 365137

Reaktionsgleichung

Reaktionsgleichung von HRID 365137
[NH:1]1[CH2:6][CH2:5][CH:4]([CH:7]2[C:13]3=[CH:14][CH:15]=[CH:16][N:12]3[CH2:11][C:10]3[CH:17]=[CH:18][CH:19]=[CH:20][C:9]=3[O:8]2)[CH2:3][CH2:2]1.Br[CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[C:30]([O-:33])([O-:32])=O.[K+].[K+].CN(C=[O:40])C>>[C:9]([OH:8])(=[O:40])[C:30]([OH:33])=[O:32].[C:24]1([CH2:23][CH2:22][N:1]2[CH2:2][CH2:3][CH:4]([CH:7]3[C:13]4=[CH:14][CH:15]=[CH:16][N:12]4[CH2:11][C:10]4[CH:17]=[CH:18][CH:19]=[CH:20][C:9]=4[O:8]3)[CH2:5][CH2:6]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

Komponenten

5

Edukt 4

HCID 6228DimethylformamideHCID 7666Phenethyl bromideHCID 11430Potassium CarbonateHCID 1368935811-(piperdin-4-yl)-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine

Produkt 1

HCID 2019167911-{1-[2-(Phenyl)ethyl]piperidin-4-yl}-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine oxalate

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

To 50 ml DMF were added 11-(piperidin-4-yl]-5H,11H-pyrrolo[2,1-c][1,4]benzoxazepine (4.5 g, 0.017 mole), (2-bromoethyl)-benzene (4.3 ml, 0.03 mole), milled K2CO3 (10.0 g, 0.07 mole) and KI (0.01 g). After stirring at 90° C. for four hours the mixture was cooled and filtered, and the filtrate was concentrated in vacuo to an oil. This oil was dissolved in ethyl acetate, washed twice with water and dried (saturated NaCl, anhydrous MgSO4).

Aufarbeitung

  1. temperaturewas cooled
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated in vacuo to an oil
  4. dissolutionThis oil was dissolved in ethyl acetate
  5. washwashed twice with water
  6. dry with materialdried (saturated NaCl, anhydrous MgSO4)

Quellen und Nachweise

ORD-Eintrag
ord-4a0197bcf38041eaa9c2b2fbe18c0959
Quelldatensatz
uspto-grants-1986_08
Patentnummer
US04608374

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