3-Chloroperoxybenzoic acid synthesis
- Product Name:3-Chloroperoxybenzoic acid
- CAS Number:937-14-4
- Molecular formula:C7H5ClO3
- Molecular Weight:172.57
618-48-4
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937-14-4
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Yield:937-14-4 98.7%
Reaction Conditions:
Stage #1: 3-chlorobenzamidewith sodium nitrite;N-bromoacetamide at 16; for 2.16667 h;
Stage #2: with zinc fluoride;water for 4 h;Temperature;
Steps:
3 A method for synthesizing a pharmaceutical intermediate of m-chloroperoxybenzoic acid comprises the following steps:
A: 2 mol of m-chlorophenylacetamide was added to the reaction vessel.900ml mass fraction of 16% sodium nitrate solution,Control the stirring speed of 260 rpm, the solution temperature to 16 ° C,Add 6mol mass fraction of 22% methyl n-butyl ether solution,6mol mass fraction of 26% 1,4-butanediol solution,6 mol of N-bromoacetamide was added in 4 portions over 40 min.Continue to react for 90 minutes;B: Then add 6 mol of aqueous solution,4mol of zinc fluoride powder,Controlling the stirring speed 330rpm, the reaction was continued 4h,Adding a mass fraction of 11% sodium chloride solution for 50 minutes,The mass fraction was washed with 37% 3-heptanol solution for 40 min.Recrystallized in a 65% nitroethane solution,Dehydrated with anhydrous sodium sulfate dehydrating agent,Inter-chloroperoxybenzoic acid to give the finished 339.528g, a yield of 98.7%.
References:
CN108239009,2018,A Location in patent:Paragraph 0016-0019; 0020-0023; 0024-0027
535-80-8
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937-14-4
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587-04-2
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937-14-4
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618-46-2
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937-14-4
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18791-75-8
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624-92-0
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222554-16-7
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937-14-4
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