Synthesis method for allicin derivative
A synthesis method and a technology of derivatives, which are applied in the field of synthesis of allicin derivatives, can solve the problems of being unsuitable for industrial production, harsh conditions, and cumbersome steps, and achieve clean and environmentally friendly reaction yields, mild reaction conditions, and high reaction yields. high effect
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Embodiment 1
[0018] Embodiment 1: Methyl methyl thiosulfinate preparation of
[0019] Dimethyl disulfide (20g) and L-proline (2g) were dissolved in acetonitrile (10ml), and hydrogen peroxide (30%, 40g) was added dropwise thereto at 0°C; stirred, and the temperature was naturally raised to 25°C, After the reaction is complete, remove acetonitrile under reduced pressure at 20°C; add dichloromethane to extract and separate layers, collect the organic layer, wash with saturated brine, and dry with anhydrous sodium sulfate; concentrate under reduced pressure at 20°C to remove the solvent , the obtained light yellow oily product is 18.7 g of methyl methyl thiosulfinate, the molar yield is 80%, and the HPLC purity is >90%.
Embodiment 2
[0020] Embodiment 2: methyl methyl thiosulfonate preparation of
[0021] Dimethyl disulfide (40g) and L-proline (4g) were dissolved in methyl tetrahydrofuran (10ml), and hydrogen peroxide (30%, 150g) was added dropwise thereto at 10°C; stirred and naturally warmed to 30 ℃, after the reaction is complete, remove methyl tetrahydrofuran under reduced pressure at 20°C; add dichloromethane to extract and separate layers, collect the organic layer, wash with saturated brine, and dry with anhydrous sodium sulfate; reduce pressure at 20°C Concentrate and remove the solvent to obtain a light yellow oily product, 46 g of methyl methyl thiosulfonate, with a molar yield of 85% and an HPLC purity of >90%.
Embodiment 3
[0022] Embodiment 3: Ethyl ethyl thiosulfinate preparation of
[0023] Diethyl disulfide (100g) and L-proline (5g) were dissolved in 1,2-dichloroethane (40ml), and hydrogen peroxide (30%, 160g) was added dropwise thereto at 10°C; stirred , raised the temperature to 40°C, after the reaction was complete, added dichloromethane to extract and separate the layers, collected the organic layer, washed with saturated brine, and dried with anhydrous sodium sulfate; concentrated under reduced pressure at 20°C, and removed the solvent to obtain The light yellow oily product was 90 g of ethyl thiosulfinate, the molar yield was 80%, and the HPLC purity was >90%.
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