9-phenanthrenylboronic acid synthesis
- Product Name:9-phenanthrenylboronic acid
- CAS Number:68572-87-2
- Molecular formula:C14H11BO2
- Molecular Weight:222.05
121-43-7
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573-17-1
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$6.00/5g
68572-87-2
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$14.00/1g
Yield:68572-87-2 82%
Reaction Conditions:
Stage #1:9-bromophenanthrene with n-butyllithium in tetrahydrofuran at -78 - 0; for 1 h;Inert atmosphere;
Stage #2:Trimethyl borate in tetrahydrofuran at -78 - 20; for 12 h;Inert atmosphere;
Stage #3: with hydrogenchloride in tetrahydrofuran;water for 0.5 h;Inert atmosphere;
Steps:
Synthesis of intermediate-3
Under nitrogen, 2.57 g (10 mmol) of 9-bromophenanthrene was dissolved in 40 ml of anhydrous THF, the temperature of the reaction was lowered to -78 ° C,After slowly adding 4 ml of 2.5 M n-BuLi dropwise, the reaction was stirred at 0 ° C for 1 hour. Then, the temperature of the reactionAfter lowering to -78 deg. C, 12.47 g (12 mmol) of trimethylborate was added dropwise, and the mixture was stirred at room temperature for 12 hours. The reactionAfter completion of the reaction, 2N-HCl aqueous solution was added, stirred for 30 minutes, and extracted with ether.Water in the organic layer was removed with anhydrous MgSO 4, filtered under reduced pressure, and then the organic solvent was concentrated to obtain a compound, Hex: EA = 4:1 to obtain 1.82 g (82%) of Intermediate-3.
References:
NANJING TOPTO MATERIALS CO., LTD.;Kim, Jin-Woo;Quin, Chao;Xu, Jun;Wang, Dening KR2017/49295, 2017, A Location in patent:Paragraph 0123-0121
5419-55-6
386 suppliers
$12.00/5g
573-17-1
327 suppliers
$6.00/5g
68572-87-2
307 suppliers
$14.00/1g
121-43-7
371 suppliers
$13.00/25mL
573-17-1
327 suppliers
$6.00/5g
7732-18-5
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$12.69/100ml
68572-87-2
307 suppliers
$14.00/1g
688-74-4
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$10.40/25mL
573-17-1
327 suppliers
$6.00/5g
68572-87-2
307 suppliers
$14.00/1g
573-17-1
327 suppliers
$6.00/5g
68572-87-2
307 suppliers
$14.00/1g