Sodium Carbonate → Tris(tris(trimethylsiloxy)silylpropyl)amine

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Reaktionsgleichung

I[CH2:2][CH2:3][CH2:4][Si:5]([O:16][Si:17]([CH3:20])([CH3:19])[CH3:18])([O:11][Si:12]([CH3:15])([CH3:14])[CH3:13])[O:6][Si:7]([CH3:10])([CH3:9])[CH3:8].[NH2:21][CH2:22][CH2:23][CH2:24][Si:25]([O:36][Si:37]([CH3:40])([CH3:39])[CH3:38])([O:31][Si:32]([CH3:35])([CH3:34])[CH3:33])[O:26][Si:27]([CH3:30])([CH3:29])[CH3:28].C(=O)([O-])[O-].[Na+].[Na+]>CC(N(C)C)=O>[CH3:8][Si:7]([CH3:10])([CH3:9])[O:6][Si:5]([CH2:4][CH2:3][CH2:2][N:21]([CH2:2][CH2:3][CH2:4][Si:5]([O:16][Si:17]([CH3:19])([CH3:18])[CH3:20])([O:11][Si:12]([CH3:15])([CH3:14])[CH3:13])[O:6][Si:7]([CH3:8])([CH3:9])[CH3:10])[CH2:22][CH2:23][CH2:24][Si:25]([O:36][Si:37]([CH3:39])([CH3:38])[CH3:40])([O:26][Si:27]([CH3:28])([CH3:29])[CH3:30])[O:31][Si:32]([CH3:35])([CH3:34])[CH3:33])([O:16][Si:17]([CH3:20])([CH3:19])[CH3:18])[O:11][Si:12]([CH3:15])([CH3:14])[CH3:13]

Komponenten

Reaktionsbedingungen

Temperatur: 80 °C

Versuchsvorschrift

14.3 g of 3-iodopropyltris(trimethylsiloxy)silane (28), 5.7 g of 3-aminopropyltris(trimethyl-siloxy)silane and 9.6 g of sodium carbonate are added to 50 ml dimethylacetamide and stirred for 15 hours at 80° C. The dimethylacetamide is then evaporated and the residue taken up in methylene chloride. The organic phase is washed with water, dried and evaporated. The product is purified by column chromatography on silica gel to give 7 g of a slightly yellowish oil of formula (30); 1H-NMR (ppm, CDCl3): 2.21 6H t, 1.38 6H txt, 0.28 6H t, 0 81H s.

Aufarbeitung

customThe dimethylacetamide is then evaporated
washThe organic phase is washed with water
customdried
customevaporated
customThe product is purified by column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag: ord-8f5669107d6e42f5a259c26cffdf9dd8
Quelldatensatz: uspto-grants-2016_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09403987B2

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