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Dimethylformamide → 3-{3-[Cyano-(5-isopropyl-2,6-dimethoxy-pyrimidin-4-yl)-methyl]-5-methyl-phenyl}-acrylonitrile

HRID 426168
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 426168
Cl[C:2]1[C:7]([CH:8]([CH3:10])[CH3:9])=[C:6]([O:11][CH3:12])[N:5]=[C:4]([O:13][CH3:14])[N:3]=1.Br[CH2:16][C:17]1[CH:18]=[C:19]([CH:24]=[CH:25][C:26]#[N:27])[CH:20]=[C:21]([CH3:23])[CH:22]=1.[H-].[Na+].[Cl-].[NH4+].[CH3:32][N:33](C=O)C>>[C:32]([CH:16]([C:2]1[C:7]([CH:8]([CH3:10])[CH3:9])=[C:6]([O:11][CH3:12])[N:5]=[C:4]([O:13][CH3:14])[N:3]=1)[C:17]1[CH:18]=[C:19]([CH:24]=[CH:25][C:26]#[N:27])[CH:20]=[C:21]([CH3:23])[CH:22]=1)#[N:33]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 5

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 160881865-Isopropyl-6-chloro-2,4-dimethoxypyrimidineHCID 667054103-(3-Bromomethyl-5-methyl-phenyl)-acrylonitrile

Produkt 1

HCID 66705650
3-{3-[Cyano-(5-isopropyl-2,6-dimethoxy-pyrimidin-4-yl)-methyl]-5-methyl-phenyl}-acrylonitrile
Ausbeute 16 %

Versuchsvorschrift

To a stirred mixture of 4-chloro-5-isopropyl-2,6-dimethoxy-pyrimidine (7.12 g, 32.88 mmol) and 3-(3-bromomethyl-5-methyl-phenyl)-acrylonitrile (5.7 g, 31.21 mmol) in anhydrous DMF (60 ml) at 0° C. (ice bath) under nitrogen atmosphere, was portionwise added 60% sodium hydride (2.76 g, 68.88 mmol). After stirring for 1 hr., the mixture was further stirred at room temperature for overnight. The mixture was then neutralized with aqueous saturated ammonium chloride solution and the crude product was extracted with ether and purified by silica gel column chromatography (eluent, EA: hexanes (from 1:4 to 1:2)) to afford 1.8 g (16%) of a pale yellow foam. 1H NMR (300 MHz, CDCl3) δ 1.12 (3H, d, J=6.9 Hz), 1.15 (3H, d, J=6.9 Hz), 2.37 (3H, s), 3.02 (1H, m), 4.01 (6H, s), 5.39 (1H, s), 5.87 (1H, d, J=16.5 Hz), 7.23 (1H, s), 7.25 (1H, s), 7.27 (1H, s), 7.33 (1H, d, J=16.5 Hz).

Aufarbeitung

  1. stirring, the mixture was further stirred at room temperature for overnight
  2. extractionthe crude product was extracted with ether
  3. custompurified by silica gel column chromatography (eluent, EA: hexanes (from 1:4 to 1:2))

Quellen und Nachweise

ORD-Eintrag
ord-121e4c55bbf04429b888af7e32f8a2dc
Quelldatensatz
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08106064B2

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