5-Chloro-2-nitroaniline synthesis
- Product Name:5-Chloro-2-nitroaniline
- CAS Number:1635-61-6
- Molecular formula:C6H5ClN2O2
- Molecular Weight:172.57
611-06-3
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Yield:1635-61-6 261.2 g
Reaction Conditions:
with ammonia at 90 - 140; under 7500.75 - 60006 Torr; for 4 h;Autoclave;Temperature;
Steps:
4-6 example 6
In a magnetic stirring autoclave, 339.2 g (99.1%, 1.75 mol) of 2,4-dichloronitrobenzene was added, and the autoclave was sealed, stirring was started, then 134.9 g (99.5%, 7.9 mol) of liquid ammonia was introduced, and the temperature was raised to 90 ° C by heating, the heating was stopped, after the temperature was stable, the temperature was controlled to 120~135 ° C, the pressure was 1.0~8.OMPa, the final temperature does not exceed 140 °C, the reaction was about 4 hours, and the pressure was released to normal pressure. In addition, 600 g of water was added in a 2000 ml beaker, and the mixture was heated to 50 to 70 ° C with stirring. After the pressure relief of the high pressure reactor was completed, the material was transferred to water while stirring, stirred for half an hour, suction filtered, and the filter cake was dried to obtain a dark yellow solid powder 308.2 g, a melting point of 117 to 119 ° C, then subject to methanol crystallization and purification, and drying, to obtain a yellow needle crystals 261.2 g, the melting point was 126.8 ° C, the content was 98.6%, and the molar yield was 85.27%.
References:
CN108329211,2018,A Location in patent:Paragraph 0017; 0019
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