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Sodium hydride → HCID 73848368, Verbindung

HRID 1737210
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1737210
[CH:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][C:2]=1[C:11](=[N:13][OH:14])[CH3:12].[H-].[Na+].[Cl:17][C:18]1[N:19]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[CH2:31]Cl)[C:20](=[O:24])[N:21]([CH3:23])[N:22]=1>CN(C)C=O.C(OCC)(=O)C>[Cl:17][C:18]1[N:19]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[CH2:31][O:14][N:13]=[C:11]([C:2]2[CH:3]=[CH:4][C:5]3[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=3[CH:1]=2)[CH3:12])[C:20](=[O:24])[N:21]([CH3:23])[N:22]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 24758Sodium hydrideHCID 240448HCID 240448, VerbindungHCID 10956231HCID 10956231, Verbindung

Produkt 1

HCID 73848368HCID 73848368, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857
Ethyl Acetate
Lösungsmittel
2×

Versuchsvorschrift

To a solution of the title compound of Step C (700 mg, 3.7 mmol) in dimethylformamide (10 mL) was added sodium hydride as a 60% oil dispersion (160 mg) followed by the title compound of Step B. The mixture was stirred at room temperature for 4 h and then was diluted with ethyl acetate. The solution was washed with water and then saturated sodium chloride solution. The organic phase was dried (MgSO4) and concentrated under reduced pressure to afford an oil. Chromatography of this oil on silica gel with 20-30% ethyl acetate in hexanes afforded 1.0 g of the title compound of Step D, a compound of the invention, as an oil which solidified on standing. 1H NMR (CDCl3): δ 7.68 (m,7H), 5.2 (m,2H), 3.47 (s,3H), 2.75 (m,4H), 2.15 (s,3H), 1.78 (m,4H). This material was used in the preparation of Example 4 without further characterization.

Aufarbeitung

  1. washThe solution was washed with water
  2. dry with materialThe organic phase was dried (MgSO4)
  3. concentrationconcentrated under reduced pressure
  4. customto afford an oil

Quellen und Nachweise

ORD-Eintrag
ord-1db286a674804a7498f6b482b84c4373
Quelldatensatz
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05962436

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