9-Phenanthreneboronic acid neopentylglycol ester synthesis
- Product Name:9-Phenanthreneboronic acid neopentylglycol ester
- CAS Number:1416371-19-1
- Molecular formula:C19H19BO2
- Molecular Weight:290.16
68572-87-2
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Yield:1416371-19-1 98%
Reaction Conditions:
in toluene at 120; for 4 h;Inert atmosphere;Dean-Stark;
Steps:
1 Comparative Example 1 Synthesis of Compound 1
Under a nitrogen stream, a 200 mL four-necked flask was charged with 9-phenanthrene boronic acid(20.0 g, 90.0 mmol), neopentyl glycol(10.3 g, 99.1 mol) and toluene (60 mL) were added,To prepare a reaction solution. Dean-Stark apparatusIt was attached to a 200 mL four-necked flask,The water generated during the reaction was separated and stirred at 120 ° C. for 4 hours.After completion of the reaction, all the solvent was distilled off. To the obtained concentrated residue was added dichloromethane(150 mL) was added, and the mixture was washed with pure water and saturated saline sequentially to separate and wash.Thereafter, the obtained organic layer was dried with anhydrous magnesium sulfate.By concentrating the organic layer and vacuum drying,25.6 g (yield 98.0%) of Compound 1 as a pale yellow powder was obtained.The GC purity of the obtained Compound 1 was measured and found to be 99.25%.
References:
JP2015/124191,2015,A Location in patent:Paragraph 0034; 0037
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