(6-phenyldibenzo[b,d]thiophen-4-yl)boronic acid synthesis
- Product Name:(6-phenyldibenzo[b,d]thiophen-4-yl)boronic acid
- CAS Number:1115640-18-0
- Molecular formula:C18H13BO2S
- Molecular Weight:304.17
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Yield:1115640-18-0 65%
Reaction Conditions:
Stage #1: 4-phenyldibenzo[b,d]thiophenewith n-butyllithium in tetrahydrofuran at -78 - 20;
Stage #2: Trimethyl borate in tetrahydrofuran at -78 - 20;
Stage #3: waterwith hydrogenchloride in tetrahydrofuran;
Steps:
2.2 2) Preparation of compound 2-2
Compound 2-1 in a 3L round flask81.2g (311.89mmol, 1eq) and driedTHF (Tetrahydrofuran)After dissolving in 1.8L, it was cooled to -78°C.After 2.5M n-ButhylLi137.2ml (343.08mmol, 1.1eq)Was added dropwise and heated to room temperature.After cooling to -78 againAfter adding trimethyl borate 42.1g (405.45mmol, 1.3eq), the mixture was heated to room temperature and stirred.After the reaction, neutralize with 1N HClIt was dissolved in ethylacetate (EA), extracted with water, and the EA layer was dried over MgSO4.After sedimentation with EA/Hexane was filtered, 61.3 g of Compound 2-2 was obtained in a yield of 65%.
References:
KR2020/68397,2020,A Location in patent:Paragraph 0174; 0179-0182
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$75.00/100mg
5419-55-6
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