Clopidol synthesis

Yield:2971-90-6 91.5%

Reaction Conditions:

Stage #1:ethyl acetoacetate at 30; for 5 h;
Stage #2: with ammonium hydroxide at 10; for 2 h;
Stage #3: with chlorine at 30; for 2 h;Reagent/catalyst;Temperature;

Steps:

2 Example 2
In three 500 ml flask, 130 g of ethyl acetoacetate (1 mole), Styrene-DVB (D301T) 39 g resin, reaction at 30 5 hours, 100 ml of distilled water, stirring the ammonia released 85 g (5 mol), reacted at 10 deg.] C after 2 hours with stirring chlorine gas at 142 g (2 mol), reacted at 30 2 hours and filtered Styrene-DVB (D301 T) and the resin solid cake was washed with NaOH (10% concentration) was washed with an aqueous solution of 100 ml, Styrene-DVB (D301T) resin is recyclable. The filtrate was distilled to remove a small amount of ethanol, allowed to stand to crystallize, filtered and dried to give the desired product 87.8 g, 91.5% yield.

References:

Zhejiang University of Technology;Pei, Wen;Sun, Li;Zhao, Dianlin;Han, Yiting;Sun, Wen CN105753776, 2016, A Location in patent:Paragraph 0009; 0020; 0021

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