Methylbutyric acid synthesis
- Product Name:Methylbutyric acid
- CAS Number:600-07-7
- Molecular formula:C5H10O2
- Molecular Weight:102.13
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Yield:600-07-7 92%
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen;acetone at 30; under 760.051 Torr;Autoclave;Industrial scale;Reagent/catalyst;Temperature;
Steps:
2 Example 2
In a 100 L autoclave were sequentially added 16.8 kg of 2-ethyl acrolein, 168 g of 10% palladium carbon, 30 kg of acetone,The reaction was replaced with nitrogen, and then three times with hydrogen,Then close the pressure relief valve, open the hydrogen inlet valve,Inflate to 1 atmosphere. Then heated to 30 °C ± 2 °C ,And this temperature insulation reaction,Until the reaction is no longer absorbed hydrogen,This process takes about 1.5 hours. TLC and GC detection reaction is completed, the reaction solution was filtered to recover palladium carbon catalyst, the filtrate was added 13.2 grams of sodium tungstate, the reaction temperature was controlled at 40 °C ± 2 °C ,Slowly drop 25% hydrogen peroxide 27.8 kg,After TLC and GC detection of the reaction was complete, sodium tungstate was filtered off,The reaction mixture was distilled to give a crude product of 99.0% purity,After the distillation column distillation separation of the desired product 2-methylButyric acid 18.8 kg, GC content 99.8%, yield 92%.
References:
CN105175247,2017,B Location in patent:Paragraph 0015-0018
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