Electric Literature of 20850-43-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 20850-43-5 name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
ake 10g about 89.7% content of piperazine pyrimidine, 12g triethylamine, 34ml isopropanol into 100ml three reaction flask, dropping peppermint chloride at room temperature under stirring, dropping over 30 minutes. Heated to 50 , incubated for 2 hours, cooled to room temperature with stirring, filtered, the mother liquor was recovered, the filter cake was added 20ml water beating, suction filtration, plus 10ml water washing cake. 50 drying, get piribedil crude 16.6g, HPLC analysis content of 99.2%. Yield 92%; 16g of crude piribedil (99.2%), 0.3g of activated charcoal and 42ml of absolute ethanol were added into a 100ml single-necked flask and heated to the reflux temperature for 0.5 hour. The activated carbon was removed by hot filtration and the filtrate was cooled and crystallized under stirring to obtain a white Crystalline solid. Filtered, rinsed with a small amount of anhydrous ethanol, and dried to obtain 14.76g of the first crystal product of piribedil, the content of which was 99.90% by HPLC and the refined yield was 90.33%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-(Chloromethyl)benzo[d][1,3]dioxole, and friends who are interested can also refer to it.
Reference:
Patent; Taicang Datang Chemical Fiber Factory; Liu Huifeng; (9 pag.)CN107266429; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics