Butyric trimethoxy

In order to elaborate the reactivity profile of compounds 3a - 3d, the rate constants of the first hydrolysis step were determined by H NMR spectroscopy (pH = 4 or 9, 30-fold molar excess H2O). In addition to the methylene-bridged silanes 3a - 3d, 3-methacryloyloxypropyl-trimethoxysilane 3e, propyl trimethoxy silane 4a, vinyl trimethoxy silane 4b, as well as butyric acid... 

Pass chlorine gas into an ice cold, well-stirred solution of 5 ml acetylketene in 30 ml CCl until there is a 4.5 g increase in weight (solution is slightly yellow). Pour slowly into excess methanol or ethanol at 0° and distill at 118/17 to get 6 ml methyl (or ethyl)-4-Cl-acetoacetate (1). To 2.7 ml methanol saturated with dry HCI at 0°, add a mixture of 10 g (I), 20 g methyl orthoformate (trimethoxy-methane) and 13 g methanol and reflux four hours. Pour hot into 200 ml ice water and adjust pH to 8 with 30% NaOH. Extract four times with ether and evaporate and distill to get methyl (or ethyl)-4-Cl-3,3-dimethoxy-butyrate (II). Dissolve 40 g (11) in 20 ml methanol and add hydroxylamine.HCI in methanol. After ninety-six hours at room temperature (under Nj if possible), evaporate in vacuum. Qan purify the residue by dissolving in water and put on anionic column wash column to neutrality and elute with 2N acetic acid just before the acid elutes, the alkaline fraction giving a positive FeClj test appears evaporate in vacuum this fraction below 40° and dry at 40/0.5 for twelve hours. Dissolve 5 g product in 130 ml glacial acetic acid and saturate at room temperature, then at 0° with dry HCI. Let stand sixteen hours at room temperature and evaporate in vacuum at 40°. Dilute with water and evaporate three times. Extract with 2X130 ml hot ether and filter, evaporate in vacuum to get 3-Cl-methyl-5-OH-isoxazole (111) (recrystallize-acetone). Heat (111) sixteen hours at 90° in concentrated NH OH in autoclave and evaporate to get muscimole. 

Both ToF-SlMS and XPS [45] have been applied to polytetrafluoroethylene (PTFE) [46,47], polybutadiene [48], rubbers [49,50], acrylics [51,52], PE [53-55], PU [56], PS [57], polyvinylcarbazole [58] polymalic acid [59], poly-P-hydroxy butyrate [60], poly-P hydroxyvalecate [60], y-glycidoxy propyl trimethoxy-silane [61], polypyrrole [62] and acrylonitrile-butadiene rubber [63]. 

---