2,2-Dichloro-1-(4-chlorophenyl)ethanone synthesis
- Product Name:2,2-Dichloro-1-(4-chlorophenyl)ethanone
- CAS Number:5157-57-3
- Molecular formula:C8H5Cl3O
- Molecular Weight:223.48
99-91-2
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Yield:5157-57-3 98%
Reaction Conditions:
Stage #1: para-chloroacetophenonewith ammonium chloride in acetonitrile; for 0.0833333 h;
Stage #2: with 1,3-dichloro-5,5-dimethylhydantoin in acetonitrile at 35; for 12 h;
Steps:
5 General procedure for preparation of α,α-dichloroacetophenone
General procedure: A mixture of 2.5 mmol of NH4Cl, 5.0 mmol of substrate, and 10.0 mL of acetonitrile was stirred for 5 min, and then 7.5 mmol of DCDMH was added by five times in 1h, and the mixture was stirred 12 h at 35°C. Afterward, solvent was distilled under reduced pressure; 20 mL of ethyl acetate was added to the residue. Next, the ethyl acetate layer was washed twice with water (20 mL), and dried over anhydrous Na2SO4. After filtration, the solvent was removed under reduced pressure, and the residue was purified by silica gel chromatography (petroleum ether/ethyl acetate=20/1, v/v) to give the product.
References:
Zheng, Zubiao;Han, Bingbing;Cheng, Peng;Niu, Jiangxiu;Wang, Aidong [Tetrahedron,2014,vol. 70,# 52,p. 9814 - 9818]
873-73-4
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27704-37-6
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28587-05-5
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706-07-0
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