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ChemicalBook CAS DataBase List Leaf alcohol
928-96-1

Leaf alcohol synthesis

13synthesis methods
By the reaction of butyne-1 with ethylene oxide and subsequent selective reduction to the eis isomer (Bedoukian, 1967).
55230-25-6 Synthesis
5,6-Dihydro-2-methyl-2H-pyran

55230-25-6
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Yield:928-96-1 97.5%

Reaction Conditions:

with 5% ruthenium on carbon;hydrogen in toluene at 100; under 15001.5 Torr; for 4 h;Autoclave;Reagent/catalyst;Temperature;Pressure;

Steps:

5-27

In a 500ml autoclave, add 100g of pretreated methylpyran, 3.0g of 5% Ru/C catalyst, 100g of toluene, the reaction temperature is 100°C, the hydrogen pressure is 2MPa, and the reaction time is 4h. After testing, the conversion rate of methylpyran was 98.64%, and the selectivity of leaf alcohol was 99.32%. The gas phase detection result is as shown in Figure 1, wherein, the retention time 6.349min is the raw material methyl pyran, the area ratio is 1.35724%, the peak retention time between 6.5 and 7.0 is the solvent toluene, and the retention time The peak of 8.591min is The product leaf alcohol accounts for 97.9677% of the area.The reaction solution was transferred to a desolvation bottle, and desolvated under the vacuum of a circulating water vacuum pump, and 95.8 g of solvent toluene was recovered. After the precipitation is completed, vacuum distillation is carried out under the vacuum of the oil pump, and the fractions are collected to obtain 100.11 g of the finished leaf alcohol, with a content of 99.4% and a yield of 97.5%.

References:

CN115073264,2022,A Location in patent:Paragraph 0035-0096

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