Synthetic method for isopropyl-beta-D-thiogalactoside
A technology of thiogalactoside and synthesis method, which is applied in the synthesis field of isopropyl-β-D thiogalactoside, can solve the problems of toxicity, unsuitability for industrial production, low yield and the like, and achieves broad market prospects , easy operation, high yield effect
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[0031] Example one
[0032] step one:
[0033] In a 500ml round flask, add 23.4g (60mmol) pentaacetylgalactose, 120ml of dichloromethane, stir to dissolve, then add 9.12g (120mmol) of thiourea into the system, stir well for 5min, add boron trifluoride ether The solution was 29.4ml (240mmol), stirred at room temperature for twelve hours, a white solid precipitated in the system, and the reaction was followed by TLC. After the reaction was complete, the white solid was filtered and recrystallized with acetone and petroleum ether to obtain pure S- Tetraacetylgalactoseisothiourea fluorinated salt was 24.5 grams, and the yield was 96%.
[0034] Step two:
[0035] Add 17.1g (90mmol) of sodium metabisulfite, 150ml of dichloromethane and 150ml of water into a 500ml round-bottomed flask, stir well, add 24.5g (57mmol) of S-tetraacetylgalactoseisothiourea fluorosalt, and heat to reflux After reacting for 6-7h, follow the reaction with TLC (petroleum ether / ethyl acetate=1:1). After the reaction...
Example Embodiment
[0040] Example two
[0041] step one:
[0042] In a 500ml round flask, add 23.4g (60mmol) pentaacetylgalactose, 120ml of dichloromethane, stir to dissolve, then add 11.4g (150mmol) of thiourea into the system, fully stir for 5min, add boron trifluoride ether The solution was 29.4ml (240mmol), stirred at room temperature for twelve hours, a white solid precipitated in the system, and the reaction was followed by TLC. After the reaction was complete, the white solid was filtered and recrystallized with acetone and petroleum ether to obtain pure S- Tetraacetylgalactoseisothiourea fluorinated salt was 25.6 grams, and the yield was 97%.
[0043] Step two:
[0044] Add 19.1g (100mmol) of sodium metabisulfite, 150ml of dichloromethane and 150ml of water into a 500ml round-bottomed flask, stir well and add 25.6g (58mmol) of S-tetraacetylgalactoseisothiourea fluorosalt, and heat to reflux , React for 6-7h, follow the reaction with TLC (petroleum ether / ethyl acetate=1:1), after the reaction i...
Example Embodiment
[0049] Example three
[0050] step one:
[0051] In a 500ml round flask, add 23.4g (60mmol) pentaacetylgalactose, 120ml of dichloromethane, stir to dissolve, then add 11.4g (150mmol) of thiourea into the system, fully stir for 5min, add boron trifluoride ether The solution was 14.9ml (120mmol), stirred at room temperature for 12 hours, and a white solid was precipitated. The reaction was followed by TLC. After the reaction was completed, the white solid was filtered and recrystallized to obtain pure S-tetraacetyl galactose isosulfide The urea fluoro salt was 19.0 grams, and the yield was 74%.
[0052] Step two:
[0053] Add 10.0g (50mmol) of sodium metabisulfite, 150ml of dichloromethane and 150ml of water into a 500ml round bottom flask, stir well and add 19.0g (44mmol) of S-tetraacetylgalactoseisothiourea fluorosalt, and heat to reflux , React for 6-7h, follow the reaction with TLC (petroleum ether / ethyl acetate=1:1), after the reaction is completed, cool to room temperature, extr...
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