Trimethyl Orthomethoxyacetate

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The electrolysis was discontinued after 10 h, when 64% of tetramethoxyethane and 76% of pentenenitrile had been converted. Trimethyl orthoformate, methyl formate and formaldehyde dimethyl acetal had formed at the anode in a ratio of 1:0.17:0.1. The main products at the cathode were 3.4-diethyladiponitrile, pentanenitrile and 3-methoxypentanenitrile in a ratio of 1:0.3:0.8. A distillative workup provided the hydrodimerization 20 product of pentenenitrile, namely 3.4-diethyladiponitrile, in 97% purity.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dimethyl 1,3-acetonedicarboxylate (20.0 g, 115 mmol) is dissolved in a solution of 1,1,1,2-tetramethoxy-ethane (23.8 g, 158 mmol) and acetic anhydride (420 mL) and the solution is heated to reflux for 4 hours. The mixture is concentrated under reduced pressure. Toluene (200 mL) is added and the solvent removed under reduced pressure to yield the title compound. the solution is heated to reflux for 4 hours The mixture is concentrated under reduced pressure Toluene (200 mL) is added the solvent removed under reduced pressure