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ChemicalBook CAS DataBase List 4-Amino-3,5-dichloroacetophenone
37148-48-4

4-Amino-3,5-dichloroacetophenone synthesis

5synthesis methods
4-Amino-3,5-dichloroacetophenone is an intermediate in the synthesis of cough antiasthmatic crepustin. It was synthesized by chlorination of 4-aminoacetophenone. Add 4-aminoacetophenone and acetic acid (80%) into the reaction pot, stir and dissolve, quickly add chlorine-containing glacial acetic acid solution, the temperature of the addition is 5 °C, after the addition is completed, immediately put into ice water to precipitate the precipitate, filter, and wash with water to obtain the crude product Recrystallize with ethanol to obtain the finished product of 3,5-dichloro-4-aminoacetophenone.
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Yield:37148-48-4 88.6%

Reaction Conditions:

with iron(III) chloride in chloroform at 0 - 20; for 6 h;

Steps:

2.1 Preparation of 3,5-dichloro-4-aminoacetophenone
A 250 mL three-necked flask was charged with 8.3 g of 2,6-dichloroaniline,After adding 50 mL of chloroform and stirring to disperse,Add ferric chloride 30g,Control temperature 0 ° C was added dropwise acetyl chloride 8.8g,After completion of the dropwise addition at room temperature for 6 hours,After acidification,Suction filtration,Washed with water to give 9.0 g of light yellow 3,5-dichloro-4-aminoacetophenone,Yield 88.6%, HPLCTesting, purity 99.5%

References:

Shanghai Chemical Institute;Xu Zhongjie;Luo Yong;Sun Kai;Yang Weicheng;Sun Wen;Li Meihua;Tu Yahui;Zhong Jiaqi;Fang Chao CN105968021, 2016, A Location in patent:Paragraph 0168-0169

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