9-broMo-8-Methoxy-6,6-diMethyl-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile synthesis
- Product Name:9-broMo-8-Methoxy-6,6-diMethyl-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile
- CAS Number:1256579-00-6
- Molecular formula:C20H17BrN2O
- Molecular Weight:381.27
17672-26-3
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1256578-99-0
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1256579-00-6
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Yield:-
Reaction Conditions:
with trifluoroacetic acid at 100; for 2 h;
Steps:
232
6-Bromo-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound E1, 7.89 g, 27.85 mmol) and 3-hydrazino-benzonitrile (4.45 g, 1.2 eq.) were dissolved in TFA (250 mL), and stirred at 100° C. for 2 hr. TFA was removed under reduced pressure and the residues were added with saturated aqueous solution of NaHCO3 (500 mL), followed by extraction with ethyl acetate. The organic layer was washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were added with ethyl acetate. After stirring at room temperature, the precipitated solid was separated by filtration (Compound E2-2). The filtrate was concentrated under reduced pressure to obtain the title compound as a mixture with E2-2 (yellowish white powder, 2.65 g).LCMS: m/z 381, 383 [M+H]+ HPLC retention time: 3.03 min (analysis condition S)
References:
US2012/83488,2012,A1 Location in patent:Page/Page column 92
1865-83-4
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$54.00/100mg
1256579-00-6
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