CHES synthesis
- Product Name:CHES
- CAS Number:103-47-9
- Molecular formula:C8H17NO3S
- Molecular Weight:207.29
Yield:103-47-9 86%
Reaction Conditions:
Stage #1: cyclohexylaminewith copper;sodium sulfite in ethanol;water;Reflux;
Stage #2: 1,2-dichloro-ethane in ethanol;water at 65; for 3 h;
Steps:
1-3 Example 2
In a 1L three-necked flask with mechanical stirring, first add 300ml of water and 400g of absolute ethanol.Stir evenly, then add 99g (1mol) cyclohexylamine, 5g copper powder,132g (1.05mol) sodium sulfite to form a mixed solution, heat the mixed solution to reflux,Then, 128g (1.3mol) 1,2-dichloroethane was slowly added dropwise, and the dropping time was controlled within 2h,After the dripping is completed, react for 1 hour at the reflux temperature of 65°C to obtain a reaction liquidThe reaction liquid is filtered to remove the catalyst copper powder, and the mother liquor is distilled under reduced pressure.Remove the mixture of ethanol and water, or recycle it for reuse;After the bottom of the distillation kettle is viscous, add 600ml of absolute ethanol to dissolve it.Adjust pH to 5-7 with concentrated hydrochloric acid, cool and crystallize to obtain a crude product,This crude product was rectified to obtain 178 g of refined product N-cyclohexyl-2-aminoethanesulfonic acid, the yield of which was about 86%, and the purity of chromatographic analysis was 99.5%.
References:
CN112479938,2021,A Location in patent:Paragraph 0015; 0033-0038
108-91-8
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103-47-9
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