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CAS No. : | 13708-12-8 | MDL No. : | MFCD00012335 |
Formula : | C9H8N2 | Boiling Point : | - |
Linear Structure Formula : | (CH3)C8H5N2 | InChI Key : | CQLOYHZZZCWHSG-UHFFFAOYSA-N |
M.W : | 144.17 | Pubchem ID : | 61670 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
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% | With 10 wtpercent sulfated polyborate; In neat (no solvent); at 100℃; for 0.05h;Green chemistry; | General procedure: To a mixture of substituted o-phenylenediamines derivative(2.0 mmol) and 1,2-diketone / alpha-hydroxy ketone (2.0 mmol),was added sulfated polyborate (10 wt%). The reaction mixture was stirred at 100 C in an oil bath. The reaction was monitored by thin layer chromatography (TLC). After completion of the reaction, the mixture was cooled to room temperature and quenched by water. The resultant product was filtered/extracted with EtOAc to get the product. Crude products were either recrystallized from ethanol or purified by column chromatography using silica as the stationary phase and EtOAc: pet. ether as mobile phase. The products obtained were known compounds and were identified by melting point and 1H and 13C NMR spectroscopy. The spectral data were compared with the literature values. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63.6% | With N-Bromosuccinimide; dibenzoyl peroxide; In 1,2-dichloro-ethane; at 110℃; for 4h; | <strong>[13708-12-8]5-Methylquinoxaline</strong> (0.180 mL, 1.387 mmol, commercially available from, for example, Sigma-Aldrich), NBS (289 mg, 1.624 mmol), benzoyl peroxide (37 mg, 0.153 mmol) and 1,2- dichloroethane (4 mL) was stirred at 110 C for 2 h. Further portions of NBS (260 mg, 1.461 mmol)and benzoyl peroxide (31 mg, 0.128 mmol) were added and the reaction refluxed for a further 2 h. The solution was concentrated to give 1.1 g of a brown solid which was purified by chromatography on 5i02 (Biotage SNAP 50 g cartridge, eluting with O-100% diethylether/cyclohexane). The desired fractions were concentrated to give 5-(bromomethyl)quinoxaline (310 mg, 0.882 mmol, 63.6 % yield) as a yellow oil.LCMS (2 mm Formic): Rt=0.91 mi [MH] = 223, 225. |
With bromine; dibenzoyl peroxide; at 70℃; for 10h; | Example 4. Synthesis of TN-5In a 250 mL three-necked bottle was placed 5-methyl quinoxaline (2.88 g, 0.02 mol), benzoyl peroxide(20 mg) was added, CC14 (80 mL) was added, then the reaction was refluxed at 70 C for 10 hrs. The product was cooled and filtered to obtain a crude 2-bromomethyl quinoxaline, the compound was not separated, an excess amount of tert-butyl amine was added, and the reaction was stirred at room temperature for 3 hrs to obtain 5-methyl tert-butylamine quinoxaline (670 mg) in a yield of 15.6%.The above-obtained compound (670 mg, 0.003 mol) were added methanol (60 mL), Na2W04 '2H20 (O.lg) and 30%> H202 (3.5 mL), the reaction was proceeded at roomtemperature for 2.5 hrs. The product was separated by column chromatography (ethyl acetate : petroleum ether = 2: 1) to obtain a light yellow compound TN-4 (154 mg) in a yield of 21.5%.1HNMR (CDC13): 1.69 (s, 9H), 7.83 (dd, IH), 8.10 (dd, IH), 8.80 (d, IH), 8.87 (d, IH), 9.19 (s, IH), 9.96 (dd, IH); ESI-MS: 230 [M+H]+; Anal. (Ci3Hi5N30) C. H. N; found C 68.04%, H 6.95%, N 18.0%; requires: C, 68.10; H, 6.59; N, 18.33. |