Industrial production process for desmethylvenlafaxine
A technology of desvenlafaxine and its production method, which is applied in the fields of organic chemistry, chemical instruments and methods, and the preparation of organic compounds, which can solve the problems of unfavorable commercial production, high reaction temperature, and high process cost, and meet the requirements of reaction conditions The effect of reduction, low price, and process cost reduction
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Embodiment 1
[0048] The industrialized production technique of desvenlafaxine, its step is as follows:
[0049] 1. Put 625.0L of dimethylformamide into the reactor at room temperature.
[0050] 2. Pass cooling water into the reactor jacket, stir and cool the dimethylformamide to 10-15°C.
[0051] 3. Put 64.2kg of sodium hydride into the reactor at 10-15°C.
[0052] 4. The reaction mass is heated to 15-20°C and stirred.
[0053] 5. Slowly put 99.0kg of ethanethiol into the reactor.
[0054] 6. After adding about 81.5L of ethanethiol, the stirring rate increased to 30-50 rpm.
[0055] 7. The reaction mass was stirred at room temperature for about 2 hours.
[0056] 8. Put 125.0 kg of venlafaxine hydrochloride into the reaction kettle at room temperature.
[0057] 9. Put 46.0L of dimethylformamide into the reaction kettle, and then raise the temperature to 25-40°C.
[0058] 10. Heat the reaction mass to 120-150°C.
[0059] 11. Sampling is sent to QC for TLC detection. (The content of v...
Embodiment 2
[0076] The industrialized production technique of desvenlafaxine, its step is as follows:
[0077] 1. Put 625.0L of dimethylformamide into the reactor at room temperature.
[0078] 2. Pass cooling water into the reactor jacket, stir and cool the dimethylformamide to 10-15°C.
[0079] 3. Put 64.2kg of sodium hydride into the reactor at 10-15°C.
[0080] 4. The reaction mass is heated to 15-20°C and stirred.
[0081] 5. Slowly put 99.0kg of ethanethiol into the reactor.
[0082] 6. After adding about 81.5L of ethanethiol, the stirring rate increased to 30-50 rpm.
[0083] 7. The reaction mass was stirred at room temperature for about 2 hours.
[0084] 8. Put 125.0 kg of venlafaxine hydrochloride into the reaction kettle at room temperature.
[0085] 9. Put 46.0L of dimethylformamide into the reaction kettle, and then raise the temperature to 25-40°C.
[0086] 10. Heat the reaction mass to 120-150°C.
[0087] 11. Sampling is sent to QC for TLC detection. (The content of ven...
Embodiment 3
[0104] The industrialized production technique of desvenlafaxine, its step is as follows:
[0105] 1. Put 625.0L of dimethylformamide into the reactor at room temperature.
[0106] 2. Pass cooling water into the reactor jacket, stir and cool the dimethylformamide to 10-15°C.
[0107] 3. Put 64.2kg of sodium hydride into the reactor at 10-15°C.
[0108] 4. The reaction mass is heated to 15-20°C and stirred.
[0109] 5. Slowly put 99.0kg of ethanethiol into the reactor.
[0110] 6. After adding about 81.5L of ethanethiol, the stirring rate increased to 30-50 rpm.
[0111] 7. The reaction mass was stirred at room temperature for about 2 hours.
[0112] 8. Put 125.0 kg of venlafaxine hydrochloride into the reaction kettle at room temperature.
[0113] 9. Put 46.0L of dimethylformamide into the reaction kettle, and then raise the temperature to 25-40°C.
[0114] 10. After heating the reaction material to 120° C. for 20 minutes, continue heating to 150° C. and continue the rea...
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