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Dimethylamine → {2-[6-(ethyloxy)-7-nitro-3,4-dihydro-1(2H)-quinolinyl]-2-oxoethyl}dimethylamine

HRID 1014298
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1014298
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[N+:14]([O-:16])=[O:15])[NH:10][CH2:9][CH2:8][CH2:7]2)[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:24][C:25](Cl)=[O:26].[CH3:28][NH:29][CH3:30].C1COCC1>ClCCl.C(=O)(O)[O-].[Na+].O>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[N+:14]([O-:16])=[O:15])[N:10]([C:25](=[O:26])[CH2:24][N:29]([CH3:30])[CH3:28])[CH2:9][CH2:8][CH2:7]2)[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 674DimethylamineHCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 89602Bromoacetyl chlorideHCID 594418676-(Ethyloxy)-7-nitro-1,2,3,4-tetrahydroquinoline

Produkt 1

HCID 59441935{2-[6-(ethyloxy)-7-nitro-3,4-dihydro-1(2H)-quinolinyl]-2-oxoethyl}dimethylamine
Ausbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 516892Sodium BicarbonateLösungsmittel

Versuchsvorschrift

A suspension of 6-(ethyloxy)-7-nitro-1,2,3,4-tetrahydroquinoline (5.0 g, 22.50 mmol) and potassium carbonate (6.22 g, 45.0 mmol) in dichloromethane (100 mL) was treated with bromoacetylchloride (2.336 mL, 28.1 mmol) and stirred for 25 minutes. Water was added and the organic layer was dried over sodium sulfate, filtered, taken to a residue under reduced pressure, redissolved in THF, and 2.0M dimethyl amine in THF (67.5 mL, 135 mmol) was added. The solution was stirred overnight, diluted with saturated sodium bicarbonate, and the organic layer was dried over sodium sulfate, filtered, taken to a residue under reduced pressure, and purified by column chromatography to afford {2-[6-(ethyloxy)-7-nitro-3,4-dihydro-1(2H)-quinolinyl]-2-oxoethyl}dimethylamine (5.8 g, 84% yield) as a pale yellow oil. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.34 (s, 1 H), 7.16 (s, 1 H), 4.17 (q, J=6.96 Hz, 2 H), 3.74 (t, J=5.62 Hz, 2 H), 3.21 (s, 2 H), 2.80 (t, J=6.32 Hz, 2 H), 2.21 (s, 6 H), 1.76-2.01 (m, 2 H), 1.33 (t, J=6.92 Hz, 3 H).

Aufarbeitung

  1. dry with materialthe organic layer was dried over sodium sulfate
  2. filtrationfiltered
  3. dissolutionredissolved in THF
  4. stirringThe solution was stirred overnight
  5. dry with materialthe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. custompurified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-b8a06e30b62f4c399796fbacd44d8fcf
Quelldatensatz
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07981903B2

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