4-Bromo-2-phenoxyaniline synthesis
- Product Name:4-Bromo-2-phenoxyaniline
- CAS Number:857594-84-4
- Molecular formula:C12H10BrNO
- Molecular Weight:264.12
2688-84-8
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857594-84-4
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Yield:857594-84-4 99%
Reaction Conditions:
with N-Bromosuccinimide in acetonitrile at -10; for 2 h;Autoclave;Large scale;
Steps:
1.3 Synthesis of 2-amino-5-bromodiphenyl ether
In a 50L double-layer cryostat equipped with mechanical stirring, 5 kg was added (due to batch reaction,A plurality of reactors are simultaneously carried out, so that the amount of the raw materials is sufficient to meet the requirements of the step. 2-Aminodiphenyl ether prepared in the above step (2), 30 L of acetonitrile, and the temperature in the autoclave is lowered to -10 ° C.4.80 Kg of N-bromosuccinimide was added in three portions, and the reaction was carried out for 2 hours.The mixture is distilled to recover acetonitrile, and then 15 L of water is added to the concentrate.15 L of dichloromethane, stirred and separated, and the organic phase was distilled to recover dichloromethane.Drying again gave a brown solid of 7.06Kg.The product was identified as 1-amino-5-bromodiphenyl ether by 1H-NMR and 13C-NMR.The yield was 99%, and the purity of the product was 98% by liquid chromatography.
References:
CN109942527,2019,A Location in patent:Paragraph 0049; 0054; 0055
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2216-12-8
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1493-27-2
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