With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.2516-33-8, name is Cyclopropylmethanol, molecular formula is C4H8O, molecular weight is 72.1057, as common compound, the synthetic route is as follows.Safety of Cyclopropylmethanol
10062] Into a clean, dry reactor equipped with a stirrer and under nitrogen are successively loaded 4.63 kg of DMF (5.1 eqV) and then 4.53 kg of triphenylphosphite. 2.34 kg of bromine is then introduced while maintaining the temperature at less than 12 C. The stirring speed is regulated according to the fluidity of the reaction medium. When casting ends, a very thick medium with a yellow solid suspension is obtained.10063] The set point of the jacket is then adjusted to -12 C. and then 0.96 kg of cyclopropylmethanol is introduced in such a way as not to exceed a temperature of -5 C. On completion of the addition the whole is allowed to return slowly to room temperature. The set point of the jacket is then adjusted to 64 C. for distillation, which is carried out at a pressure of 13 mbar by collecting the first 24 to 30 C. fraction at the top of the colunm, then the second 30 to 40 C. fraction (partial reflux). Two fractions, Fl (1.38 kg) and F2 (293 g), are collected. The two fractions, after washing with carbonated water and then drying by means of CaC12, lead to a final product 2a (mass 1.316 kg) having a GC relative purity of 98.7% with a yield of 73%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,2516-33-8, Cyclopropylmethanol, and friends who are interested can also refer to it.
Reference:
Patent; MELCHIOR MATERIAL AND LIFE SCIENCE FRANCE; GUERRET, Olivier; (6 pag.)US2016/355452; (2016); A1;,
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