106966-25-0 Usage
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).
Check Digit Verification of cas no
The CAS Registry Mumber 106966-25-0 includes 9 digits separated into 3 groups by hyphens. The first part of the number,starting from the left, has 6 digits, 1,0,6,9,6 and 6 respectively; the second part has 2 digits, 2 and 5 respectively.
Calculate Digit Verification of CAS Registry Number 106966-25:
(8*1)+(7*0)+(6*6)+(5*9)+(4*6)+(3*6)+(2*2)+(1*5)=140
140 % 10 = 0
So 106966-25-0 is a valid CAS Registry Number.
106966-25-0Relevant articles and documents
Preparation method for high-purity 3-(2,2,2-trimethylhydrazine)methyl propionate crude drug intermediate
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Paragraph 0012; 0014, (2019/03/08)
The invention discloses a preparation method for a high-purity 3-(2,2,2-trimethylhydrazine)methyl propionate crude drug intermediate. The intermediate is an important medical intermediate of mildronate and aziridine anti-cancer drugs. A conventional method is that 1,1-dimethylhydrazine reacts with methyl acrylate, and vacuum distillation is performed and a methylation reaction is performed to obtain a target product. The intermediate obtained by this type of the reaction contains ammonium salt related impurities so that the variety and content of final crude drug impurities exceed an impuritylimited field of European Pharmacopoeia, and a purifying technology is complicated. The invention provides an efficient improved method for preparing the two types of the compounds. A high-purity product can be obtained and a productive rate of the product is improved, cost is reduced, and industrial large-scale production is realized.
