The preparation method of 1-p-menthene-8-thiol
A technology for menthene and mercaptans, applied in the field of fine chemistry, can solve problems such as unsuitability for industrial production, expensive and dangerous lithium tetrahydrogen, and complicated synthetic routes, and achieve shortened production cycles, optimized synthetic routes, and simple operations Effect
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Embodiment 1
[0040] A kind of preparation method of 1-menthene-8-mercaptan, comprises the following steps:
[0041] S1, add 1kg a-terpineol to the reactor, add 6L THF, and stir until completely dissolved;
[0042] S2. Add 1kg of phosphorus pentasulfide in batches to the solution obtained in step S1, with temperature rise, and the temperature is controlled below 50°C;
[0043] S3, react at 50°C for 1 hour, monitor the GC by gas phase, and the reaction is completed;
[0044] S4. The reacted system was lowered to room temperature, and the THF was removed by rotary evaporation for recycling, and 6L of 10% sodium hydroxide aqueous solution was slowly added to pH ≥ 12;
[0045] S5. Extract the aqueous phase twice with tertiary methyl ether, 3 L each time, combine the organic phases and wash with saturated brine once, 1 L each time, dry with anhydrous sodium sulfate, concentrate to obtain 1 kg of crude product, and distill under reduced pressure to obtain 400 g of product 1- For Menthene-8-thio...
Embodiment 2
[0047] A kind of preparation method of 1-menthene-8-mercaptan, comprises the following steps:
[0048] S1, add 1kg a-terpineol to the reactor, add 4L DMF, stir until completely dissolved;
[0049] S2. Add 1kg of phosphorus pentasulfide in batches to the solution obtained in step S1, with temperature rise, and the temperature is controlled below 50°C;
[0050] S3, react at 50°C for 1 hour, monitor the GC by gas phase, and the reaction is completed;
[0051] S4. Lower the reacted system to room temperature, and slowly add 6L of 10% sodium hydroxide aqueous solution to pH ≥ 12;
[0052] S5. Extract the aqueous phase twice with tertiary methyl ether, 3 L each time, combine the organic phases and wash with saturated brine once, 1 L each time, dry with anhydrous sodium sulfate, concentrate to obtain 1.1 kg of crude product, and distill under reduced pressure to obtain 410 g of product 1 - p-mentene-8-thiol, GC purity >85%.
Embodiment 3
[0054] A kind of preparation method of 1-menthene-8-mercaptan, comprises the following steps:
[0055] S1, add 1kg a-terpineol to the reactor, add 6L THF, and stir until completely dissolved;
[0056] S2. Add 1.85kg Lawesson's Reagent in batches to the solution obtained in step S1, with temperature rise, and the temperature is controlled below 50°C;
[0057] S3, react at 50°C for 1 hour, monitor the GC by gas phase, and the reaction is completed;
[0058] S4. The reacted system was lowered to room temperature, and the THF was removed by rotary evaporation for recycling, and 6L of 10% sodium hydroxide aqueous solution was slowly added to pH ≥ 12;
[0059] S5. Extract the aqueous phase twice with tertiary methyl ether, 3 L each time, combine the organic phases and wash with saturated brine once, 1 L each time, dry with anhydrous sodium sulfate, concentrate to obtain 700 g of crude product, and distill under reduced pressure to obtain 300 g of product 1- p-menthene-8-thiol, GC ...
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