Synthesizing method of 3-sulfonyl alcohol compounds
A synthesis method and compound technology are applied in the field of 3-sulfone-based alcohol compounds and the green synthesis field of catalyst-free water solvent, which can solve the problem that the method has not been reported by anyone.
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Embodiment 1
[0018] Example 1: Take a 38 mL thick-walled pressure-resistant tube, weigh p-toluenesulfonyl hydrazide (0.5 mmol, 96.8 mg) into it, and then add a solution of allyl alcohol (1 mmol, 0.12 mL) into it, the solvent For 1mL of water, add a suitable type of magnet, and check whether the rubber gasket of the sealing plug is intact. Then, tighten the screws of the sealing tube, and heat and react in an oil bath at 80° C. for 11 hours. Stop heating, cool down to room temperature naturally, slowly unscrew the stopper, extract the reaction solution with EtOAc (50 mL×3), combine the organic phase, wash the organic phase with saturated brine, collect the organic phase, and dry over anhydrous sodium sulfate for half an hour , The solvent was removed by rotary evaporation to obtain 3-p-toluenesulfonylpropanol, 82.31 mg of white crystal powder, and the yield was 76.9%. 1 HNMR (400 MHz, CDCl 3 ) δ7.81 (d, J = 8.3 Hz, 2H), 7.39 (d, J = 8.0 Hz, 2H), 4.33 (s, 1H), 3.45–3.38(m, 2H), 2.83–2.77 (...
Embodiment 2
[0019] Example 2: Take a 15 mL thick-walled pressure-resistant tube, weigh benzenesulfonyl hydrazide (1.5 mmol, 258.3 mg) and add it, then measure allyl alcohol (3 mmol, 0.36 mL) solution and add it, the solvent is 2 mL Water, add the appropriate type of magnet, check whether the rubber gasket of the sealing plug is in good condition. Then, tighten the screws of the sealing tube, and heat the reaction in an oil bath at 100°C for 10h. Stop heating, cool down to room temperature naturally, slowly unscrew the stopper, extract the reaction solution with EtOAc (50 mL×3), combine the organic phase, wash the organic phase with saturated brine, collect the organic phase, and dry over anhydrous sodium sulfate for half an hour , The solvent was removed by rotary evaporation to obtain 3-benzenesulfonylpropanol, 249.31 mg of white crystal powder, and the yield was 83%.
Embodiment 3
[0020] Example 3: Take a 38mL thick-walled pressure-resistant tube, weigh p-nitrobenzenesulfonyl hydrazide (1mmol, 217.2 mg) into it, then measure allyl alcohol (1.4 mmol, 0.16 mL) solution into it, add 2mL of water Make a solvent, add a suitable type of magnet, and check whether the rubber gasket of the sealing plug is intact. Then, tighten the screw of the sealing tube, and heat the reaction in an oil bath at 60° C. for 5 hours. Stop heating, cool down to room temperature naturally, slowly unscrew the stopper, extract the reaction solution with EtOAc (50 mL×3), combine the organic phase, wash the organic phase with saturated brine, collect the organic phase, and dry over anhydrous sodium sulfate for half an hour , The solvent was removed by rotary evaporation to obtain 3-nitrobenzenesulfonyl propanol, 198.65 mg of white crystal powder, and the yield was 81%.
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