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CAS No. : | 1086378-35-9 | MDL No. : | MFCD11042246 |
Formula : | C9H7NO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | SVWYSYMOKICPBK-UHFFFAOYSA-N |
M.W : | 177.16 | Pubchem ID : | 19771047 |
Synonyms : |
|
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: |
* 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 |
---|---|---|
98.2% | With toluene-4-sulfonic acid; for 0.5h;Inert atmosphere; Reflux; | General procedure: The compound obtained in Example 32-1 (400 mg, 3.20 mmol) triethyl orthoformate (3.2 ml, 19.2 mmol) in solution,para-tosylic acid monohydrate(30 mg, 0.16 mmol) was added dropwise. Under an argon atmosphere, followed by stirring for 30 minutes under reflux conditions, it was solidified after completion of the reaction concentrated to dryness. The residue was purified by silica gel column chromatography (hexane / ethyl acetate) to give the title compound (232 mg, 54%) |
Example XV Methyl 2-benzoxazole-7-carboxylate STR34 5.8 ml of CCl4 in 5 ml of acetonitrile were added to 30 mmol of the compound from Example XIV, 30 mmol of benzoic acid, 50 mmol of triphenylphosphine and 120 mmol of triethylamine in 100 ml of acetonitrile at 3 C. under argon in the course of 15 min and the mixture was stirred at room temperature for 20 hours and concentrated, diethyl ether was added to the residue, the solid was filtered off with suction, the filtrate was concentrated and the residue was separated on silica gel. M.p.: 77 C. (white needles) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With copper(l) iodide; palladium diacetate; caesium carbonate; 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In toluene; for 20.0h;Inert atmosphere; Reflux; | General procedure: To a degassed solution (N2 was purged for 10 min) of methyl 1,3-benzoxazole-4-carboxylate (150 mg, 0.847mmol) and N-(2-iodophenyl)benzamide 2a (273 mg, 0.847 mmol) in anhydrous toluene (4ml) , CuI (32 mg, 0.169 mmol), xantphos (98 mg, 0.169 mmol), Pd(OAc)2 (10 mg, 0.042 mmol), Cs2CO3 (685 mg, 2.117 mmol) were added at room temperature under nitrogen atmosphere. Reaction mixture was continued for 20 hours at reflux condition. After the completetion of the reaction (monitored by TLC), Reaction mixture was filtered through celite bed and washed with methanol (10 ml),filtrate was concentrated. Crude mass which was purified by column chromatography over silica gel (230-400 mesh) using DCM-Methanol (1:9) as elutant to affordthe products 3a (284 mg) as white solid. All the other compounds 3b-3r were prepared similarly following the above procedure. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | With ytterbium(III) triflate; In toluene; at 100℃; for 1.0h;Microwave irradiation; | Methyl 3-amino-2-hydroxybenzoate (1.69 g, 10.13 mmol) was suspended in toluene (2 mL) in a microwave vial. HC(OEt)3 (1.80 g, 12.15 mmol) and Yb(OTf)3 (0.003 g, 0.005 mmol) was added and the reaction was heated at 100 C for 1 hour in the microwave. The reaction mixture was evaporated and purified by flash chromatography (petroleum ether/EtOAc 4:1) to give the title compound (1.63 g, 91%) as pale yellow crystals. mp. 116 - 118 C (Litt9. 77 C). 1H NMR (300 MHz, CDCl3) delta 8.21 (s, 1H), 8.04 (dd, J = 7.8, 1.2 Hz, 1H), 7.99 (dd, J = 8.0, 1.2 Hz, 1H), 7.44 (dd, J = 8.0, 7.8 Hz), 3.76 (s, 3H). 13C NMR (75 MHz, CDCl3) delta 180.9, 164.4, 153.4, 141.4, 128.0, 125.6, 124.5, 115.4, 52.6 |
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