Reaktionsgleichung
[C:1]([O-:4])(=[O:3])[CH3:2].[K+].Cl[CH2:7][SiH2:8][CH:9]([O:12][CH3:13])[O:10][CH3:11]>[Br-].C([P+](CCCC)(CCCC)CCCC)CCC.C(OCCOCCOCCCC)CCC>[C:1]([O:4][CH2:7][SiH2:8][CH:9]([O:12][CH3:13])[O:10][CH3:11])(=[O:3])[CH3:2]Komponenten
Versuchsvorschrift
Example 2 was repeated using potassium acetate (405 g, 4.13 mol) and (chloromethyl)dimethoxymethylsilane (535 g, 3.46 mol) as starting materials, tetrabutylphosphonium bromide (35.0 g, 10.3 mmol) as catalyst and diethylene glycol dibutyl ether (525 mL) as solvent. After the reaction, the product was distilled at 10 mbar (head), 61-70° C. (head) and 80-119° C. (pot) through a packed column (20 cm) to obtain 560 g (3.14 mol, 91% of theory) of (acetoxymethyl)-dimethoxymethylsilane in the distillate; purity 98.0% (GC area %). The solvent then started to pass over at 10 mbar (head), 118° C. (head) and 124° C. (pot); by distilling over about 10 g of solvent, the (acetoxymethyl)dimethoxymethylsilane was fully removed from the residue. The solvent, potassium chloride, excess potassium acetate and the phase transfer catalyst (in the form of the bromide, chloride and acetate salt of tetrabutylphosphonium) remained in the residue.
Aufarbeitung
- customAfter the reaction
- distillationthe product was distilled at 10 mbar (head), 61-70° C. (head) and 80-119° C. (pot) through a packed column (20 cm)
Quellen und Nachweise
- ORD-Eintrag
- ord-1ae6698a9fea467c960df6ac1a9893dd
- Quelldatensatz
- uspto-grants-2014_04
- Patentnummer
- US08692012B2
Verknüpfte Notizen
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