1-Ethynyl-1-cyclohexanol synthesis
- Product Name:1-Ethynyl-1-cyclohexanol
- CAS Number:78-27-3
- Molecular formula:C8H12O
- Molecular Weight:124.18
Yield:78-27-3 91 %
Reaction Conditions:
Stage #1: cyclohexanonewith n-butyllithium in tetrahydrofuran;hexane at -10 - 0;Inert atmosphere;
Stage #2: trimethylsilylacetylene in tetrahydrofuran at 25;Inert atmosphere;Temperature;
Steps:
1-3 Example 1
Add 100g of cyclohexanone and600g of solvent tetrahydrofuran,mix and dissolve,After that, nitrogen replacement was performed three times,Then, under stirring,And dropwise add 400mL of n-butyllithium solution (2.5M n-hexane) at the temperature of -10-0°C, After the dropwise addition, the insulation was carried out to react for 1 hour. get the reaction solution; Add 110g ofTrimethylsilylacetylene, Afterwards, the reaction system was heated to 25° C. for 2 hours,After the reaction is over, cool the system down to a temperature of 0-5°C and add water.Quenching the reaction to obtain a mixture;Then directly carry out vacuum distillation to above-mentioned mixture,And collect the fraction of 65-69 (1000Pa),gives ethynylcyclohexanol,Its purity is greater than 99%,The yield is 91%;
References:
CN115521190,2022,A Location in patent:Paragraph 0050-0070
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