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CAS No. : | 479-27-6 | MDL No. : | MFCD00004033 |
Formula : | C10H10N2 | Boiling Point : | - |
Linear Structure Formula : | (NH2)2C10H6 | InChI Key : | YFOOEYJGMMJJLS-UHFFFAOYSA-N |
M.W : | 158.20 | Pubchem ID : | 68067 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
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* 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 |
---|---|---|
91% | With copper(l) iodide; In 1,4-dioxane; at 150℃; for 1h;Microwave irradiation; | General procedure: A mixture of 1a (50 mg, 0.18 mmol), 1,8-diaminonaphthalene (2) (41.5 mg, 0.26 mmol), and CuI (3.3 mg, 0.018 mmol) in dioxane (1.0 mL) was stirred for 60 min at 150 C under microwave irradiation (300 W). The reaction mixture was concentrated under reduced pressure and purified by column chromatography over silica gel with hexane-EtOAc (15:1). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
27% | With zinc acetate hydrate; In methanol; at 20℃; for 16h;Inert atmosphere; | To a stirred solution of compound 39 (0.3 g, 1.82 mmol) inmethanol (5 mL) was added a solution of naphthalene-1,8-diamine (0.24 g, 1.52 mmol) in methanol(5 mL). Then Zn(OAc)2 (0.028 g, 0.128 mmol) was added and the mixture was stirred at roomtemperature for 16 h. The reaction mixture was filtered, the filter cake was washed with methanol,dried to get compound 40 (125 mg, 27percent), mp 92.3?94.8 °C. 1H-NMR (DMSO-d6) delta: 3.88 (s, 3H), 5.50(s, 1H), 6.54 (d, J = 7.6 Hz, 2H), 6.98 (d, J = 8.0 Hz, 2H), 7.08 (s, 2H), 7.16 (dd, J = 7.6 Hz, 8.0 Hz,2H), 7.67 (d, J = 8.0 Hz, 1H), 8.31 (dd, J = 2.0 Hz, 8.0 Hz, 1H), 9.08 (d, J = 2.0 Hz, 1H); MS (ESI):m/z calcd. for C18H16N3O2 [M+H]+ 306.1, found: 306.2. |
27.3% | With zinc acetate dehydrate; In methanol; at 20℃; | A mixture of 1,8-naphthalenediamine (0.24 g, 1.52 mmol)Was dissolved in methanol (5 mL)A solution of compound 26 (0.3 g, 1.82 mmol) in methanol was slowly added,After adding,Zinc acetate (0.028 g, 0.128 mmo 1) was added,Stirred at room temperature overnight,After completion of the reaction,Take the filter,washing,Drying and other measures to get the compound27 (150 mg,27.3percent) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88% | In methanol; for 6h;Reflux; | 1,8-diaminonaphthalene (3.0 g, 18.9 mmol,Tokyo Chemical Industry Co., Ltd.),9-Dulolidine carboxaldehyde (3.8 g, 31.6 mmol,Tokyo Chemical Industry Co., Ltd.) was dissolved in methanol (24 ml)And the mixture was stirred under heating reflux for 6 hours.After cooling to room temperature,The precipitate was collected by filtration,To give an intermediate product 1-d (5.7 g, yield 88.0%).Then,The resulting intermediate product 1-d (5.6 g, 16.4 mmol),Potassium carbonate (7.25 g, 52.4 mmol),A mixture of 1-iodobutane (10.56 g, 57.3 mmol) and N, N-dimethylformamide (56 ml) was placed in a 100 C. oil bath,And the mixture was heated and stirred for 6 hours.Water (56 ml) was added,Quench,The precipitate was collected by filtration,Purification by recrystallization,To obtain a compound (5.1 g, yield 68.5%) represented by the formula (6d). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78.1% | With zinc acetate dehydrate; In methanol; at 20℃; for 15h; | A solution of <strong>[67808-64-4]methyl 5-formylthiophene-2-carboxylate</strong> 39 (645 mg, 3.79 mmol), 1,8-naphthalenediamine (500 mg,3.16 mmol), Zinc acetate dihydrate (58 mg,0.265 mmol) was dissolved in methanol (5 mL)The reaction was carried out at room temperature for 15 h,TLC test raw material reaction is completed.During the reaction, solid precipitates,The reaction solution was filtered,To give compound 40 (764.8 mg, 78.1percent) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
73% | In ethanol; for 5h;Reflux; | General procedure: In ethanolic solution,a mixture of 1,8-diaminonaphthalene 6 (0.40 g, 2.5 mmol)and ethyl aroyl pyrovate 10 (2.5mmol) was reuxed for 5 hrs. The reaction mixture was allowed to cool at room temperature,and then, the solid formed was collected by filltration,dried, and recrystallized from ethanol. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91.5% | In dimethyl sulfoxide; toluene; for 12h;Inert atmosphere; Molecular sieve; Dean-Stark; Reflux; | Under an argon atmosphere,(4-methyl-3-nitrophenyl) boronic acid (3.62 g, 20 mmol),1,8-diaminonaphthalene (4.8 g, 15 mmol)And 4mg molecular sieves 500mgIs dimethyl sulfoxide,Mixed solution of toluene55 mL (1:10 (v / v))Dissolved inRefluxed in the Dean-Stark apparatus for 12 hours.After confirming the completion of the reaction by thin-layer chromatography (also referred to as “TLC”),The reaction solution was cooled to around room temperature.Add 30 mL of water to the reaction solution,Extracted three times with 30 mL of ethyl acetate.The organic layer is dried over anhydrous magnesium sulfate (also called "MgSO4"),The solvent was distilled off.The residue was purified by silica gel column chromatography using n-hexane / ethyl acetate = 1/1 as an eluent to give compound (41).(5.55 g, 91.5% |
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