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CAS No. : | 194851-16-6 | MDL No. : | MFCD07838323 |
Formula : | C8H5BrN2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | FUGKKMYSCAYXJJ-UHFFFAOYSA-N |
M.W : | 225.04 | Pubchem ID : | 135555612 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-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 |
---|---|---|
71% | With trifluoroacetic acid; In ISOPROPYLAMIDE; at 160℃; for 0.5h;Microwave radiation; | To a solution of <strong>[112253-70-0]2-amino-4-bromo-benzamide</strong> (1 equiv) in DMA (0.14 M) were added triethyl orthoformate (10 equiv) and trifluoroacetic acid (1 equiv). The reaction vessel was sealed and exposed to microwave radiation (160 0C, medium absorption setting) for 30 minutes. The reaction mixture was concentrated in vacuo and the residue was filtered through a silica pad with 10 % methanol in ethyl acetate yielding the required product as a pale yellow solid. <n="121"/>7-Bromo-3H-quinazolin-4-one: (71 % yield, 100 % purity) m/z (LC-MS, ESP): 268 [M+H]+ R/T = 2.94 min |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
84% | With sodium methylate; In ethanol; for 1.5h;Heating / reflux; | 2) 4-Bromoanthranilic amide (40 g, 186 mmol) obtained in 1) was dissolved in ethanol (400 mL). Thereto was added sodium methoxide (54.2 g, 93 mmol) with stirring under ice-cooling and then ethyl formate (60.1 mL, 744 mmol) was added dropwise. The mixture was heated under reflux for 1.5 hrs. The reaction mixture was allowed to cool to room temperature and water (500 mL) was added and then acetic acid (40 mL) was added. The mixture was concentrated under reduced pressure and water (200 mL) was added. The precipitate was collected by filtration and dried to give 7-bromo-3H-quinazolin-4-one (35 g, 156 mmol, 84%). 7-bromo-3H-quinazolin-4-one [0153] 1H NMR (DMSO-d6) delta ppm: 7.68 (dd, J=1.7, 8.5 Hz, 1H), 7.88 (d, J=1.7 Hz, 1H), 8.03 (d, J=8.5 Hz, 1H), 8.14 (s, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With [Cp*Ir(2,2'-bpyO)(H2O)]; caesium carbonate; at 130℃; for 2h;Microwave irradiation; Inert atmosphere; | 2-Amino-4-bromobenzamide (107 mg, 0.5 mmol), [Cp * Ir (2,2'-bpyO) (H2O)](5.4 mg, 0.005 mmol, 1 mol%),Cesium carbonate (49 mg, 0.15 mmol, 0.3 equiv.) And methanol (0.5 ml) were sequentially added to a dried 5 mL microwave reaction tube.The tube was nitrogen protected and placed in a single mode pressure microwave synthesizer (Discover CEM, USA). After the reaction mixture was reacted at 130 C for 2 hours, it was cooled to room temperature. Rotary evaporation to remove the solvent,Pure target compound was then obtained by column chromatography (developing solvent: petroleum ether / ethyl acetate), yield: 80% |
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