Isopropyl-beta-D-thiogalactoside preparation technology
A technology for thiogalactoside and preparation process, which is applied in the field of preparation technology of isopropyl-β-D-thiogalactoside, and achieves the effects of saving operation cost and materials, simple operation and easy availability of raw materials
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[0024] a) Add 6 mol of acetic anhydride and 1.5 mol of aluminum trichloride at room temperature, add 1 mol of galactose in 12 batches at 5-10°C, add 1.3 mol of isopropyl mercaptan after the reaction is completed, and obtain 0.774 mol of isopropyl mercaptan after the reaction is completed Propylthioacetylgalactose;
[0025] b) Add 0.774 mol of isopropylthioacetylgalactose to 10 mol of methanol to dissolve, add 0.01 mol of sodium methoxide, add 0.01 mol of acetic acid to neutralize after the reaction is completed, and obtain 0.756 mol of isopropyl-β-D- Thiogalactosides. The yield was 75.6%.
[0026] The post-treatment in step a is to dropwise add 10 mol of water at 0-5°C and stir for 2 hours, extract the aqueous layer with 5 mol of dichloromethane, separate the organic phase and wash the organic phase with 10 mol of water three times, separate the organic phase and concentrate, add 1mol tert-butyl methyl ether and 2mol isohexane mixed solution crystallized, filtered and dried....
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