3-Methyl butynol synthesis
- Product Name:3-Methyl butynol
- CAS Number:115-19-5
- Molecular formula:C5H8O
- Molecular Weight:84.12
Yield:115-19-5 99.2%
Reaction Conditions:
with sodium in methanol at 0 - 5; for 1 h;Autoclave;Inert atmosphere;Large scale;Solvent;Reagent/catalyst;
Steps:
2 Example 2 Preparation of methylbutynol
In a 500 L stainless steel autoclave, 300 L of anhydrous methanol was added under nitrogen. Under the jacketed chilled brine, 20 kg of sodium metal block was slowly added. After all the sodium metal was dissolved, add 55 L of acetone, stir well, and cool to below 0 °C. The acetylene is slowly introduced, and the flow rate of the acetylene is controlled so that the reaction temperature is 0-5 ° C. When the reaction is no longer exothermic, the reaction is complete. Then, a small amount of acetylene was introduced, and the micro-positive pressure reaction was closed for 1 hour. In another 1000 L glass-lined reactor, 150 kg of ammonium chloride, 300 L of methanol were added. The reaction solution was pumped into an ammonium chloride system to carry out a neutralization reaction under cooling with chilled brine. The neutralization reaction temperature was controlled to be less than 20 °C. After the neutralization is completed, it is filtered. The filtrate was first distilled with methanol, methanol was applied, and then the product methylbutynol was distilled under reduced pressure to obtain 62 kg. The purity of the product was 99.4%, and the yield was 99.2%.
References:
Panjin Ge Linkaimo Technology Co., Ltd.;Gong Ningrui CN108863717, 2018, A Location in patent:Paragraph 0036; 0037; 0038; 0039; 0040; 0041; 0042
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