1-Carboxy-3-MethacryloyloxyadaMantane synthesis
- Product Name:1-Carboxy-3-MethacryloyloxyadaMantane
- CAS Number:212580-10-4
- Molecular formula:C15H20O4
- Molecular Weight:264.32
79-41-4
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42711-75-1
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212580-10-4
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Yield:212580-10-4 22 g
Reaction Conditions:
with sulfuric acid;4-methoxy-phenol in toluene at 110; for 4 h;Dean-Stark;Solvent;Reagent/catalyst;Temperature;
Steps:
2
As a reaction apparatus, a stirrer, a thermometer,Dean · Starck tube,To a glass 500 mL flask equipped with Dimroth,19.6 g (100 mmol) of 3-hydroxyadamantane-1-carboxylic acid, 98 g of toluene, 25.8 g (300 mmol) of methacrylic acid,0.98 g (10 mmol) of sulfuric acid and 62 mg (0.5 mmol) of p-methoxyphenol were charged, and the temperature of the reaction solution was heated under reflux at 110 ° C. for 4 hours. When the progress of the reaction was confirmed by GC, the conversion of 3-hydroxyadamantane-1-carboxylic acid was 98% and 3- (methacryloyloxy) adamantane-1-carboxylic acid was produced with a reaction yield of 52%. After cooling the reaction vessel to 20 ° C. or lower by an ice bath, 50 g of toluene and 400 g of 5% sodium hydroxide aqueous solution were added and stirred for 1 hour. After completion of stirring, the mixture was allowed to stand for 5 minutes and subjected to liquid separation operation. To the organic layer after liquid separation, a 5% sodium hydroxide aqueous solution 100G was added and after stirring for 5 minutes, it was allowed to stand for 5 minutes and then subjected to liquid separation operation. While stirring the obtained aqueous layer, 65 g of 85% phosphoric acid was added thereto, whereby a clay-like mixture containing 3-methacryloyloxyadamantane-1-carboxylic acid was precipitated. The clay-like mixture was filtered to obtain 22 g of a solid containing 3-methacryloyloxyadamantane-1-carboxylic acid. The purity of 3-methacryloyloxyadamantane-1-carboxylic acid in the solid was HPLC-RI 60%.
References:
JP2016/84313,2016,A Location in patent:Paragraph 0082
42711-75-1
310 suppliers
$5.00/1g
212580-10-4
8 suppliers
$165.00/500mg
768-95-6
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$10.00/5g
212580-10-4
8 suppliers
$165.00/500mg
828-51-3
430 suppliers
$10.00/5g
212580-10-4
8 suppliers
$165.00/500mg