Preparation method of 9-aminoacridine and derivatives thereof
An aminoacridine and derivative technology, which is applied in the field of preparation of 9-aminoacridine and its derivatives, can solve the problems affecting the long-term operation of the device, high operational safety requirements, and many reaction by-products, etc., to ensure long-term operation. , Improve the operational safety factor, the effect of short synthesis route
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Embodiment 1
[0044] The preparation method of the 9-aminoacridine and its derivatives of the present embodiment comprises the following steps:
[0045]
[0046] Add 200g (0.94mol) of 9-chloroacridine and 435ml of DMF (N,N-dimethylformamide) into the reactor equipped with a thermometer and a stirrer, stir at room temperature, and the ammonia gas passes through the pressure reducing valve and the constant pressure The valve was passed into the reactor at a flow rate of 30L / h, and the temperature was slowly raised to 70°C, and the mixture was incubated and reacted for 3h under an ammonia atmosphere. TLC confirmed the reaction end point, and about 64L of ammonia gas was used, and DMF was recovered under reduced pressure (recovery rate 80%), lower the temperature to 40°C, add 2L of water, adjust the pH to 14 with sodium hydroxide at room temperature, stir for 10 minutes, filter, wash with water until neutral, and dry to obtain 165g of 9-aminoacridine, a yellow powder, and the separation yield...
Embodiment 2
[0049] The preparation method of the 9-aminoacridine and its derivatives of the present embodiment comprises the following steps:
[0050]
[0051]Add 200 g (0.94 mol) of 9-chloroacridine and 580 ml of N-methylpyrrolidone (NMP) into a reactor equipped with a thermometer and a stirrer, and stir at room temperature. The flow rate of h is passed into the reactor, slowly warming up to 80 ℃, and the mixture is incubated and reacted for 3.5h under methylamine atmosphere, TLC confirms the reaction end point, uses about 85L of methylamine, reclaims NMP under reduced pressure (recovery rate is 85%) ), cooled to 30°C, added 2L of water, adjusted the pH to 14 with sodium hydroxide at room temperature, stirred for 20min, filtered, washed with water until neutral, dried to obtain 181g of N-methyl-9-acridinamine, yellow powder, separated The yield was 92%, and the purity was 99.3%.
Embodiment 3
[0053] The preparation method of the 9-aminoacridine and its derivatives of the present embodiment comprises the following steps:
[0054]
[0055] Add 200 g (0.94 mol) of 9-chloroacridine and 725 ml of DMF to the reactor equipped with a thermometer and a stirrer, stir at room temperature, and feed ethylamine into the reactor at a flow rate of 30 L / h through a pressure reducing valve and a pressure stabilizing valve In the process, slowly raise the temperature to 100°C, and keep the mixture under the atmosphere of ethylamine for 4h, TLC confirms the reaction end point, uses about 105L of ethylamine, recovers DMF under reduced pressure (the recovery rate is 85%), cools to 40°C, and adds water 2L, adjust the pH to 14 with sodium hydroxide at room temperature, stir for 30 minutes, filter, wash with water until neutral, and dry to obtain 200g of N-ethyl-9-acridinamine, a yellow powder, with an isolated yield of 95% and a purity of 99.0%.
[0056] The product that present embod...
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