Yield:3685-84-5 68 g

Reaction Conditions:

Stage #1:2-(N,N-dimethylamino)ethanol;4-chlorophenyloxyacetyl chloride in dichloromethane at 20;Green chemistry;
Stage #2: with hydrogenchloride in ethyl acetateGreen chemistry;Solvent;

Steps:

1-10 Example 2
50 g (0.26 mol) of p-chlorophenoxyacetic acid was placed in dichloromethane in a single-mouth bottle.After that, 47.5 g (0.40 mol) of thionyl chloride was added dropwise, and the mixture was added dropwise, and the reaction was stirred under reflux. The reaction solution was dried to give an oil. Dichloromethane was added to the obtained oil, and a solution of 26 g (0.28 mol) of dimethylaminoethanol in dichloromethane was added dropwise to the reaction flask.After 30 minutes of dropwise addition, the reaction was stirred at room temperature. Water was added for extraction and the resulting organic layer was dried. The obtained oil was added to 250 ml of ethyl acetate, and hydrogen chloride gas was used to form a hydrochloride salt, and the solid was precipitated in a large amount, and the mixture was filtered at 25 ° C.Obtained 68 g of a white solid.Yield 87.1%, purity 99.9% (Figure 2):

References:

Guangdong South China Pharmaceutical Group Co., Ltd.;Guangdong Xian Qiang Pharmaceutical Co., Ltd.;Tan Zhenyou;Li Wan;Shang Wei CN109400489, 2019, A Location in patent:Paragraph 0035-0040; 0041; 0044

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