Yield:35139-68-5 1.368 g

Reaction Conditions:

with 3-chloro-benzenecarboperoxoic acid;sodium hydroxide in water;ethyl acetate at 0 - 25;

Steps:

3 Example 3: Synthesis of impurity formula VI.-3 compound

Add 100ml of ethyl acetate, 3.0g of impurity VI.-1 compound and 2ml of purified water to the reaction flask in turn, stir and cool down to 0~10 °C. Add 6.0g of m-chloroperoxybenzoic acid dropwise dissolved in 20ml of ethyl acetate solution, add dropwise to 20~25 °C reaction, cool down to 0~10 °C after the reaction, add 7% sodium hydroxide aqueous solution to cool down to 0~10 °C crystallization for 3h, filter the cake and add 15ml of purified water to 60 °C to beat for 1h, cool down to 20~30 °C crystallization for 1h, filter the filter cake with 5ml of water, 55 °C vacuum drying to obtain 1.368g solid.

References:

CN115572265,2023,A Location in patent:Paragraph 0071-0072