Uses
3-(2,2,2-Trimethylhydrazine)methylpropionate bromide can be used as organic synthesis intermediates and pharmaceutical intermediates, mainly used in laboratory research and development processes and chemical production processes.
Synthesis
In a three-necked round bottom flask equipped with a mechanical stirrer, a dropping funnel and a reflux condenser, 172 g (2 mol) of methyl acrylate was added, and under cooling, 132 g (2.2 mol) of 1,1-dimethylhydrazine was added dropwise. After a period of 2 hours, the reaction mixture was heated at the same temperature until methyl 3-(2,2-dimethylhydrazo)propionate was formed (monitored by GM-MS). The above methyl 3-(2,2-dimethylhydrazinyl)propanoate product was dissolved in 40% ethanol (350 ml), cooled to 0 ° C, and methyl bromide (189 g, 1.99 mol) was passed for 1 hour, and the temperature was continued. After stirring for 0, 5 hours, the yellow or brown precipitate was filtered off, and the crude product was washed with acetone (1000 ml). The crude 3-(2,2,2-trimethylhydrazine) propionate methyl bromide was dried (265.7 g, yield 91.0%); the crude product was recrystallized from ethanol and dried to give 219.8 g of pale yellow crystalline powder. The rate is 75.3%, the melting point is 130-132°C, and the main content is 103.3%. (The stability is verified by the stability test. The stability is poor, the color gradually becomes deeper. Because the trace impurities contained in the product have a great influence on the product, it is found to have molecular decay and various indicators. Larger, the product is valid for up to two years).
