10-Brom-phenanthren-9-ol synthesis
- Product Name:10-Brom-phenanthren-9-ol
- CAS Number:4120-76-7
- Molecular formula:C14H9BrO
- Molecular Weight:273.12
484-17-3
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Yield:4120-76-7 78%
Reaction Conditions:
with N-Bromosuccinimide;diisopropylamine in dichloromethane at 20; for 4 h;
Steps:
Synthesis of Intermediate I-10
5.8 g (30.0 mmol) of phenanthren-9-ol, 5.25 g (29.5 mmol) of N-bromosuccinimide (NBS), and 4.2 mL (33.0 mmol) of diisopropylamine were dissolved in 100 mL of dichloromethane, and the mixture was stirred at room temperature for 4 hours. A small amount of diluted sulfuric acid aqueous solution was added to the reaction mixture, and extraction was performed three times using dichloromethane. The collected extracted organic layer was dried over MgSO4 and then filtered, and the residual solid obtained by evaporating the solvent was separation-purified by silica gel column chromatography to obtain 6.4 g (yield of 78%) of Intermediate I-10. The obtained compound was confirmed by LC-MS and 1H NMR. C14H9BrO: M+1 273.0
References:
US2017/244048,2017,A1 Location in patent:Paragraph 0390; 0391-0392
5085-74-5
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4407-00-5
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84-11-7
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85-01-8
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