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CAS No. : | 773873-77-1 | MDL No. : | MFCD06203728 |
Formula : | C10H8BrNO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MFOKOKHNSVUKON-UHFFFAOYSA-N |
M.W : | 254.08 | Pubchem ID : | 285091 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338-P310 | 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 |
---|---|---|
62% | With sulfuric acid; for 5h;Reflux; | General procedure: 4 g of 5-substituted indole- 3- carboxylic acids was dissolved in 10 volumes(400 mL) of methanol and catalytic amount of conc.H2SO4 was added slowly. The total reaction mixture was refluxed over 5 h time period and the reaction mixture was cooled to room temperature slowly. Now ice cold water was added and the yellow color solid was filtered. This solid was recrystallized from ethanol yielded 5 -substituted -3- carbomethoxyindoles 12a-b. Methyl-5-bromo-1H-indole-3-carboxylate (12b) yellow color solid. yield 62%. m.p: 210-212 C; IR (KBr): 3213, 3114, 2929, 1745 cm-1; 1H NMR (400 MHz, CDCl3): delta 3.93 (3H, s, -OCH3), 7.28 (1H, d, J = 8.8 Hz, Ar-H),7.35 (1H, m, Ar-H), 7.91 (1H, d, J = 2.8 Hz, Ar-H), 8.32 (1H, s, Ar-H), 8.67 (1H, s, -NH) ppm; 13C NMR (400 MHz, CDCl3+ DMSO-d6): delta 49.93, 105.91, 112.88, 113.75, 122.40, 124.26, 126.65, 131.89, 134.33, 164.13 ppm; HRMS calculated for C10H9NO2Br: 253.98112; found: 253.98102. |
62% | With sulfuric acid;Reflux; | General procedure: 4 g of 5-substituted indole e 3 e carboxylic acids were dissolvedin 10 vol (400 mL) of methanol and a catalytic amount of conc.H2SO4 was added slowly. The reaction mixture was refluxed for 5 hand then cooled to room temperature. Ice cold water was addedand the product was filtered when yellow colored solid was obtained.This solid on recrystallization from ethanol yielded 5 esubstituted -3- carbomethoxy indoles 21a-21b. |
With thionyl chloride; at 20℃; for 12h; | To a solution of <strong>[10406-06-1]5-bromo-1H-indole-3-carboxylic acid</strong> (5.2 g) in MeOH (50 mL) is added dropwise thionylchloride (3.15 mL). The mixture is stirred for 12 h at room temperature. The solvent is evaporated in vacuo and the residue triturated with diethylether. The precipitate is collected by filtration to give the title compound. LC (Method 1): tR=0.94 min; Mass spectrum (ESI1): m/z=254/256 (Br) [M+H]+. |
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