18066-68-7, 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. 18066-68-7 name is Ethyl 2-(3,4-dimethoxyphenyl)acetate, 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.
(ii) 19.3 g (0.19 mol) of dried isopropylamine was dissolved in 100 ml of anhydrous tetrahydrofuran. The solution was cooled to -60 C. or below in a dry ice/acetone bath, and 120 ml of a solution of 1.6M n-butyllithium in n-hexane was dropwise added thereto at this temperature with stirring. The mixture was stirred for 15 min, and a solution of 40.37 g (0.18 mol) of ethyl 3,4-dimethoxyphenylacetate in 200 ml of anhydrous tetrahydrofuran was dropwise added thereto at the same temperature. After stirring for additional 15 min, a solution of 38.45 g (0.18 mol) of 2-chloro-3-methoxy-beta-nitrostyrene in 400 ml of anhydrous tetrahydrofuran was dropwise added thereto with stirring at such a dropping rate that the temperature of the system did not exceed -50 C. After stirring for 30 min, a small amount of water was added thereto and tetrahydrofuran was distilled off to some extent in vacuo. A 6N hydrochloric acid solution was added to the residue for acidification, and the acidified residue was extracted twice with dichloromethane. The resultant organic phase was washed twice with a saturated saline solution and dried over anhydrous magnesium sulfate. The solvent was distilled off in vacuo, and the residue was purified by silica gel column chromatography (eluted with a n-hexane/ethyl acetate mixture in a n-hexane to ethyl acetate ratio of 2:1) to prepare 75.1 g of viscous crude ethyl 3-(2-chloro-3-methoxyphenyl)-2-(3,4-dimethoxyphenyl)-4-nitrobutyrate.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 2-(3,4-dimethoxyphenyl)acetate, and friends who are interested can also refer to it.
Reference:
Patent; Eisai Co., Ltd.; US5444083; (1995); A;,
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