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

HRID 979332Notizen

Reaktionsgleichung

[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

Edukt 4

HCID 6228Dimethylformamide

HCID 7666Phenethyl bromide

HCID 11430Potassium Carbonate

HCID 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

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

Quellen und Nachweise

ORD-Eintrag: ord-ad12396a629a4e78a44aa4c882af9208
Quelldatensatz: uspto-grants-1987_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04667039

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