While the job of a research scientist varies, most chemistry careers in research are based in laboratories, where research is conducted by teams following scientific methods and standards. , Electric Literature of 3416-57-7
2.0g of compound I is mixed with 3.76g of potassium carbonate thoroughly, then the resulting mixture is poured into a 25ml flask followed by adding 4.0ml of chloroacetone into, heating the solution to 90-110C (a reflux condensing tube is needed to be equipped on the flask, the system is protected with argon) while stirring, maintaining the temperature, and conducting the reaction for 3-4 hours. After the reaction is completed, excess chloroacetone is removed under a reduced pressure, into the residue is added a great deal of water, then filtrated with Buchner’s filter. The resulting solid is washed twice with 10ml of 10% NaOH and 5-6 times with water respectively, dried under vacuum to obtain compound II; After a reflux condensing tube and a dropping funnel are connected on a three-necked bottle, 100ml of absolute methanol (or other anhydrous solvent) is added into the three-necked bottle, followed by slowly adding 0.23g of metallic sodium (or directly adding 10mmol of sodium methoxide). After the solid dissolves entirely, the solution is heated and refluxed, then compound II dissolved in absolute methanol (60ml CH3OH and 1.0g compound II) is dropped into by dropping funnel. After conducting the reflux for 2 hours the reaction is processed as follows: cooling the system with icewater bath, slowly neutralizing the reaction solution with 1M hydrochloride, continuing to stir for 30min in icewater bath after a large amount of solid emerge, filtrating to obtain a solid, then washing the solid with small amount of water, drying in vacuum, thereby obtaining compound III. 230mg of compound III is placed in a 25ml flask followed by adding 5ml solvent (listed in the above) into, air is blown into by a bubbler continuously. The reaction is completed after 10 hours and processed as follows: diluting the reaction solution with 30ml of acetic ether, extracting with water, back-extracting the water phase with 30ml of acetic ether, washing the organic phases with water and saturated salt solution respectively, combining the organic phases, then drying, condensing, the residue is applied on silica gel column (petroleum ether: acetic ether=2:1) to obtain compound IV
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Reference:
Patent; Shanghai Institute of Materia Medica, Chinese Academy of Sciences; EP1640367; (2006); A1;,
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