Synthetic process for amino aromatic hydrocarbon compound
A technology of aromatic compounds and aminoaromatics, which is applied in the field of synthesis of aminoaromatic compounds, can solve the problems of producing highly toxic nitrogen oxides, spending a lot of money to recover nitric acid, endangering biological health, etc., achieving fast speed, improving purity and yield , the effect of high industrial safety
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Embodiment 1
[0048] (1) Preparation of nitration reaction solution:
[0049] Reaction solution-1: Weigh 78g of benzene as reaction solution-1;
[0050] Reaction solution-2: Weigh 96.9g (65%) of nitric acid and 78.8g (98%) of concentrated sulfuric acid and mix, keep the temperature of the mixing process not exceeding 15°C, and use it as reaction solution-2;
[0051] (2) Synthesis of nitrobenzene:
[0052] Keep the temperature of the micro-reactor at 20°C, add the reaction solution-1 and the reaction solution-2 into the micro-reactor through the syringe pumps-1 and -2 respectively, the flow rate of the reaction solution-1 is 20mL / min, the flow rate of the reaction solution-2 The flow rate is 22 mL / min, and at this time, the molar ratio of nitric acid to benzene added is 1.05:1. After the reaction was complete, 236g of water was added and filtered to obtain 113.2g of nitrobenzene product. The nuclear magnetic resonance spectrum data of described nitrobenzene compound is as: 1 HNMR (500MHz...
Embodiment 2
[0058] (1) Preparation of nitration reaction solution:
[0059] Reaction solution-1: weigh 165g of p-acetamidoanisole and mix with 825g (98%) concentrated sulfuric acid as reaction solution-1;
[0060] Reaction solution-2: Weigh 67.0g (95%) nitric acid as reaction solution-2;
[0061] (2) Synthesis of 2-nitro-4-acetamidoanisole:
[0062] Keep the temperature of the microreactor at 50°C, and add the reaction solution-1 and the reaction solution-2 into the microreactor through the syringe pumps-1 and -2 respectively, the flow rate of the reaction solution-1 is 10mL / min, and the flow rate of the reaction solution-2 The flow rate is 95mL / min, at this time, the molar ratio of nitric acid to benzene added is 1.01:1. After the reaction was completed, 3300 g of water was added and filtered to obtain 205.8 g of 2-nitro-4-acetamidoanisole product. The NMR spectrum data of the 2-nitro-4-acetamidoanisole compound are as follows: 1 HNMR (500MHz, CDCl 3 ): δ1.62(s,2H), 4.20(s,3H), 7.42...
Embodiment 3
[0068] Reaction solution-1: Weigh 108g of anisole as reaction solution-1;
[0069] Reaction solution-2: Weigh 63g (95%) nitric acid and 108g (98%) concentrated sulfuric acid and mix, keep the temperature during the mixing process not exceeding 15°C, and use it as reaction solution-2;
[0070] (2) Synthesis of nitroanisole:
[0071] The temperature of the microreactor was kept at 10°C, and the reaction solution-1 and the reaction solution-2 were added to the microreactor through the syringe pumps-1 and -2 respectively. The flow rate of the reaction solution-1 was 10mL / min, and the flow rate of the reaction solution-2 was The flow rate was 9.5mL / min. At this time, the molar ratio of nitric acid and anisole was 1:1. After the reaction was completed, 324g of water was added and filtered to obtain 150g of mixed nitroanisole product.
[0072] (3) Preparation of reduction reaction solution
[0073] Reaction solution-3: Mix 150g of mixed nitroanisole obtained in the previous step wi...
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