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CAS No. : | 6373-46-2 | MDL No. : | MFCD00025318 |
Formula : | C13H13NO | Boiling Point : | - |
Linear Structure Formula : | C6H4C6H5CH2ONH2 | InChI Key : | FIIDVVUUWRJXLF-UHFFFAOYSA-N |
M.W : | 199.25 | Pubchem ID : | 22860 |
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 |
---|---|---|
In acetonitrile; for 18h;Heating / reflux; | (4-Benzyloxyphenyl)-(6-iodoquinazolin-4-yl)-amine hydrochloride 4-Chloro-6-iodoquinazoline (8 g) was treated with 4-benzyloxyaniline (5.5 g) in acetonitrile (500 ml) at reflux under N2 for 18 hours. Subsequent cooling and filtration gave the title compound (13.13 g); δH [2H6]-DMSO 11.45 (1H, b, NH), 9.22 (1H, s, 5-H), 8.89 (1H, s, 2-H), 8.36 (1H, d, 7-H), 7.69 (1H, d, 8-H), 7.63 (2H, d, 2'-H, 6'-H), 7.52-7.29 (5H, m, Ph-H), 7.14 (2H, d, 3'-H, 5'-H), 5.18 (2H, s, CH2); m/z (M+1)+ 454. | |
In acetonitrile; for 18h;Heating / reflux; | 4-Chloro-6-iodoquinazoline (8 g) was treated with 4-benzyloxyaniline (5.5 g) in acetonitrile (500 ml) at reflux under N2 for 18 hours. Subsequent cooling and filtration gave the title compound (13.13 g); δH [2H6]-DMSO 11.45 (1H, b, NH), 9.22 (1H, s, 5-H), 8.89 (1H, s, 2-H), 8.36 (1H, d, 7-H), 7.69 (1H, d, 8-H), 7.63 (2H, d, 2'-H, 6'-H), 7.52-7.29 (5H, m, Ph-H), 7.14 (2H, d, 3'-H, 5'-H), 5.18 (2H, s, CH2); m/z (M+1)+454. | |
13.13 g | In acetonitrile; for 18h;Reflux; Inert atmosphere; | (4-Benzyloxyphenyl)-(6-iodoquinazolin-4-yl)-amine hydrochloride (0637) 4-Chloro-6-iodoquinazoline (8 g) was treated with 4-benzyloxyaniline (5.5 g) in acetonitrile (500 ml) at reflux under N2 for 18 hours. Subsequent cooling and filtration gave the title compound (13.13 g); δH [2H6]-DMSO 11.45 (1H, b, NH), 9.22 (1H, s, 5-H), 8.89 (1H, s, 2-H), 8.36 (1H, d, 7-H), 7.69 (1H, d, 8-H), 7.63 (2H, d, 2′-H, 6′-H), 7.52-7.29 (5H, m, Ph-H), 7.14 (2H, d, 3′-H, 5′-H), 5.18 (2H, s, CH2); m/z (M+1)+ 454. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Example 1331-ethyl-6-fluoro-3-{4-[(3-methyl-3H-imidazo[4,5-b]pyridin-2-yl)oxy]phenyl}-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one 133a) N2-[4-(benzyloxy)phenyl]-5-fluoropyridine-2,3-diamine A mixture of 4-(benzyloxy)aniline (2.26 g), <strong>[136888-21-6]2-chloro-5-fluoro-3-nitropyridine</strong> (2 g) and K2CO3 (3.13 g) in DMF (20 ml) was stirred at 120 C. for 5 h, treated with water, and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was suspended in IPE and collected by filtration. The obtained solid was dissolved in EtOH (20 ml), and Pt/C (2 g) was added. Under H2 atmosphere, the mixture was stirred for 1 h, filtered and evaporated. The residue was chromatographed on silica gel eluting with Hexane/AcOEt to give the title compound (0.85 g).1H NMR (300 MHz, DMSO-d6) delta 5.04 (2H, s), 5.39 (2H, s), 6.69-6.80 (1H, m), 6.86-6.94 (2H, m), 7.29-7.50 (8H, m), 7.54 (1H, s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium carbonate; In N,N-dimethyl-formamide; at 120℃; for 5h; | Example 132; 1-ethyl-6-fluoro-3-{4-[(1-methyl-1H-benzimidazol-2-yl)oxy]phenyl}-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one 132a) N2-[4-(benzyloxy)phenyl]-5-fluoropyridine-2,3-diamine A mixture of 4-(benzyloxy)aniline (2.26 g), <strong>[136888-21-6]2-chloro-5-fluoro-3-nitropyridine</strong> (2 g) and K2CO3 (3.13 g) in DMF (20 mL) was stirred at 120 C. for 5 h, treated with water, and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated in vacuo. The residue was suspended in IPE and collected by filtration. The solid obtained above was dissolved in EtOH (20 ml), and Pt/C (2 g) was added. Under H2 atmosphere, the mixture was stirred for 1 h, filtered and evaporated. The residue was chromatographed on silica gel eluting with Hexane/AcOEt to give the title compound (0.85 g).1H NMR (300 MHz, DMSO-d6) delta 5.04 (2H, s), 5.39 (2H, s), 6.69-6.80 (1H, m), 6.86-6.94 (2H, m), 7.29-7.50 (8H, m), 7.54 (1H, s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
20% | With bromine; In formic acid; acetic acid; at -3 - 0℃;Inert atmosphere; Darkness; | General procedure: The synthesis of 6-ethoxy-1,3-benzothiazol-2-amine (1c), obtained following a general procedure for the preparation of aminobenzothiazoles described in the literature [13,14] is described. Aniline 6c (1.0 g, 7.36 mmol) and NH4SCN (1.6 g, 21.9 mmol) were dissolved in a 20% formic acid-glacial acetic acid mixture (100 mL) and cooled to-3 C with stirring, under N2. With the exclusion of light from the reaction mixture, bromine (0.30 mL dissolved in 20 mL of glacial acetic acid) was added dropwise, while the reaction temperature was kept between -3C and 0 C. The light shield was removed and the mixture was allowed to warm to room temperature overnight. Sodium hydroxide pellets and ice were added with stirring until pH 11 was attained, and the mixture was extracted with EtOAc. The organic layer was separated and filtered through celite to remove polythiocyanogen (SCN)n. The organic layer was then washed with water, saturated NaHCO3 and brine; then, the solvent was evaporated in vacuo. The residue was purified by flash chromatography (EtOAc/petroleum ether 1:1) to give 0.93 g (65%) of an orange solid: |
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