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CAS No. : | 203395-59-9 | MDL No. : | MFCD09753615 |
Formula : | C13H14BrNO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | MBOHAVAGDOGRBS-UHFFFAOYSA-N |
M.W : | 296.16 | Pubchem ID : | 10756315 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
98.99% | With 2,3-dicyano-5,6-dichloro-p-benzoquinone; In tetrahydrofuran; at 20℃; for 12h;Inert atmosphere; | To a 500 mL two-neck round-bottom flask fitted with a magneticstir bar and argon inlet was charged <strong>[129722-34-5]7-[4-bromobutoxy]-3,4-dihydro-2(1H)-quinolinone</strong> 5b (10 g, 0.033 mol) in THF(200 mL). To the aforementioned mixture 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (30.4 g, 0.13 mol) was added and the contents were stirred at rt until the completion of the reaction.Upon the consumption of starting material (as indicatedby TLC), THF was evaporated under reduced pressure. Theresidual product obtained was washed with water (200 mL)and extracted with ethyl acetate (3 × 100 mL). The organiclayer was washed with brine, dried over anhydrous Na2SO4,and concentrated under reduced pressure to furnish the crudeproduct. The crude product was purified by column chromatographyusing Ethyl acetate and n-Hexane as solventsystem to afford the title compound 8b.Yield: 98.99% (9.8 g);1H NMR (400 MHz, DMSO-d6) delta 11.57 (s, 1H), 7.77 (d,J = 9.4 Hz, 1H), 7.53 (d, J = 9.4 Hz, 1H), 6.83-6.69 (m,2H), 6.27 (d, J = 9.6 Hz, 1H), 4.02 (t, J = 6.1 Hz, 2H), 3.59(t, J = 6.6 Hz, 2H), 2.03-1.89 (m, 2H), 1.89-1.74 (m, 2H);13C NMR (100 MHz, DMSO-d6): delta 162.67, 160.72, 141.05,140.44, 129.69, 118.97, 113.77, 111.19, 99.05, 67.28, 35.26,29.46, 27.74; ESI (MS): 296 [M+H]+; HPLC purity: 99.26%[RT: 11.545 min; UV detection at 210 nm; Column: X BridgeC-18, 150 × 4.6 mm, 5 mum particle size; Mobile phase: A)0.1% TFA in water, B) Acetonitrile; T/%B: 0/10, 3/10, 15/95,23/95, 25/10, 30/10; Flowrate: 1.0 mL/min;Diluent:Acetonitrile:Water (80:20)]. 1H NMR spectral data of 8b was foundto be consistent with the values reported in Ref. 16. |
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