The preparation method of nevirapine
A technology of nevirapine and crude product, applied in the field of preparation of nevirapine, can solve the problems of large amount of diethylene glycol dimethyl ether, complicated operation and high boiling point of diethylene glycol dimethyl ether
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Embodiment 1
[0090] Add toluene 200ml, 2-chloro-N-(2-chloro-4-methyl-3-pyridyl)-3-pyridinecarboxamide (100.0g, 0.35mol), triethylamine (100ml, 0.72 mol), cyclopropylamine (51.0ml, 0.74mol), start stirring. Slowly raise the temperature to 130°C, and keep the reaction for 10 hours. After taking a sample to detect the remaining raw materials <2%, turn off the stirring, pass condensed water into the kettle to lower the temperature to room temperature, and obtain 2-cyclopropylamino-N-(2-chloro-4-methyl-3-pyridyl)- 3-Pyridinecarboxamide reaction mixture.
[0091] Open the autoclave, pour the above mixture into a reaction flask, add 100ml of diethylene glycol dimethyl ether, stir, cool down to 15°C, add sodium amide (44.0g, 1.13mol), and keep stirring for 10 minutes. Heat slowly to 110° C., and keep the reaction for 2 hours. After the raw materials were detected by TLC, the toluene was distilled off under reduced pressure. The residue was cooled to 20°C, 500ml of water was added dropwise, and...
Embodiment 2
[0094] Add 50ml of toluene, 2-chloro-N-(2-chloro-4-methyl-3-pyridyl)-3-pyridinecarboxamide (10.0g, 0.035mol), triethylamine (12.0ml, 0.086mol), cyclopropylamine (5.0ml, 0.072mol), start stirring. Slowly raise the temperature to 135°C, and keep the reaction for 13 hours. After taking a sample to detect the remaining raw materials <2%, turn off the stirring, pass condensed water into the kettle to lower the temperature to room temperature, and obtain 2-cyclopropylamino-N-(2-chloro-4-methyl-3-pyridyl)- 3-Pyridinecarboxamide reaction mixture.
[0095] Open the autoclave, pour the above mixture into a reaction flask, add 15ml of diethylene glycol dimethyl ether, stir, cool down to 5°C, add potassium tert-butoxide (10.0g, 0.089mol), and keep stirring for 15 minutes. Heating is slowly raised to 100° C., and the reaction is kept for 3 hours. After the raw materials were detected by TLC, the toluene was distilled off under reduced pressure. The residue was cooled to 20°C, 60ml of w...
Embodiment 3
[0098] In the autoclave, add xylene 40ml, 2-chloro-N-(2-chloro-4-methyl-3-pyridyl)-3-pyridinecarboxamide (10.0g, 0.035mol), diisopropylethylamine (12.5ml, 0.072mol), cyclopropylamine (6.0ml, 0.087mol), and start stirring. Slowly raise the temperature to 125°C, and keep it warm for 8 hours. After taking a sample to detect the remaining raw materials <2%, turn off the stirring, pass condensed water into the kettle to lower the temperature to room temperature, and obtain 2-cyclopropylamino-N-(2-chloro-4-methyl-3-pyridyl)- 3-Pyridinecarboxamide reaction mixture.
[0099]Open the autoclave, pour the above mixture into a reaction flask, add 20ml of diethylene glycol dimethyl ether, stir, cool down to 10°C, add sodium methoxide (7.5g, 0.14mol), and keep stirring for 15 minutes. Heat slowly to 115° C., and keep the reaction for 5 hours. After the reaction of raw materials was detected by TLC, xylene was distilled off under reduced pressure. The residue was cooled to 20°C, 60ml of ...
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