Methyl 2-benzoylbenzoate synthesis
- Product Name:Methyl 2-benzoylbenzoate
- CAS Number:606-28-0
- Molecular formula:C15H12O3
- Molecular Weight:240.25
131-11-3
659 suppliers
$14.00/25g
100-58-3
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$18.00/10ml
606-28-0
315 suppliers
$8.00/25g
1159-86-0
67 suppliers
$37.38/250mg
Yield:606-28-0 60% ，1159-86-0 5%
Reaction Conditions:
in tetrahydrofuran;diethyl ether at -78 - 40; for 17 h;Inert atmosphere;Temperature;
Steps:
2 EXAMPLE 2
A 3-neck 250 mL round bottom flask was charged with dimethyl phthalate (1 .0 equivalence) and tetrahydrofuran (cone. 0.2 M) under nitrogen atmosphere and phenyl magnesium bromide (1 .0 equivalence) was slowly added to the reaction mixture at -78 °C. The reaction was kept at -78 °C for an hour. After 2h, TLC and GC-FID showed mostly starting material and the reaction was warmed up to 0 °C. The reaction was kept running at 0 °C for another 3 h. TLC showed product formation, however the majority was still starting material. The reaction was slowly warmed up to 40 °C and kept running for another 12 h. After that, reaction was quenched by adding 1 N HCI solution to the reaction mixture. Diethyl ether was added and the reaction mixture was transferred to a separatory funnel. The organic layer was separated and the aqueous layer was further washed with diethyl ether. The organic layers were combined and dried over MgSC>4. The solvent was removed under reduced pressure to yield a brownish oil which was purified by silica gel chromatography (10%-25% ethyl acetate in hexane) to yield the product methyl 2-benzoylbenzoate (60% yield) and diketone product (5% yield).
References:
WO2021/168072,2021,A1 Location in patent:Paragraph 0028
131-11-3
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$14.00/25g
100-59-4
273 suppliers
$42.00/0.25mole
606-28-0
315 suppliers
$8.00/25g
1159-86-0
67 suppliers
$37.38/250mg
201230-82-2
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610-97-9
432 suppliers
$9.00/1g
603-33-8
255 suppliers
$30.00/5g
606-28-0
315 suppliers
$8.00/25g
