Vinyltriethoxysilane → HCID 19070348, Verbindung

HRID 1955496

Reaktionsgleichung

Reaktionsgleichung von HRID 1955496
[CH3:1][C:2]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)([CH3:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=[O:4].[CH:20]([Si:22]([O:29][CH2:30][CH3:31])([O:26][CH2:27][CH3:28])[O:23][CH2:24][CH3:25])=[CH2:21]>C1(C)C=CC=CC=1>[CH3:13][C:2]([N:14]1[CH2:15][CH2:16][O:17][CH2:18][CH2:19]1)([CH3:1])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][C:6]=1[CH2:21][CH2:20][Si:22]([O:23][CH2:24][CH3:25])([O:26][CH2:27][CH3:28])[O:29][CH2:30][CH3:31])=[O:4]

Komponenten

4

Edukt 2

HCID 6516VinyltriethoxysilaneHCID 923872-Methyl-1-(4-(methylthio)phenyl)-2-morpholino-1-propanone

Produkt 1

HCID 19070348HCID 19070348, VerbindungAusbeute 6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

11.18 g (40 mmol) of 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone, 735 mg (0.8 mmol) of RuH2 (CO) (PPh3)3 and 10.0 ml (48 mmol) of vinyltriethoxysilane in 60 ml of anhydrous toluene were degase with argon for 1/2 hour and boiled at reflux for 50 hours. Concentration and chromatography (silica gel, CH2Cl2 /ethyl acetate) gave 1.02 g (6%) of a yellowish oil. 1H-NMR (CDCl3): 0.99 ppm (2H, mc, Et-H2); 1.22 ppm (6H, s, CH3); 1.24 ppm (9H, t, CH3 of Si(OEt)3); 2.50 ppm (3H, s, SCH3); 2.59 ppm (4H, mc, morpholine-N--CH2); 2,69 ppm (2H, mc, Et-H1); 3.70 ppm (4H, mc, morpholine-O--CH2); 3.85 ppm (6H, q, SiOCH2, 3JH,H =6.8 Hz); 7.03 ppm (1H, dd, Ph-H5, 3 JH5,H6 =8.2 Hz, 4JH3, H5 =2.0 Hz); 7.13 ppm (1H, d, Ph-H3); 8.40 ppm (1H, d, Ph-H6).

Aufarbeitung

  1. customfor 1/2 hour
  2. temperatureat reflux for 50 hours
  3. concentrationConcentration and chromatography (silica gel, CH2Cl2 /ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-9f068ee15758499b97745354df0a50d8
Quelldatensatz
uspto-grants-1998_07
Patentnummer
US05776658

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