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CAS No. : | 17288-32-3 | MDL No. : | MFCD11053752 |
Formula : | C10H10N2O2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | NOWHXIDXMNNYBL-UHFFFAOYSA-N |
M.W : | 190.20 | Pubchem ID : | 11579250 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338-P310 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | |
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 |
---|---|---|
61% | With N-Bromosuccinimide; In dichloromethane; at 0 - 20℃; for 16h; | N-Bromosuccinimide (15.4 g, 86.5 mmcl) was added to a 0 °C solution of ethyl 1 H-pyrrolo[3,2-b]pyridine-2-carboxylate (15.0 g, 78.9 mmol) in dichloromethane (150 mL), and the reaction mixture was stirred at room temperature for 16 hours. Afteraddition of dichloromethane (150 mL) and water (200 mL), the aqueous layer was extracted with dichloromethane (3 x 150 mL). The combined organic layers were washed with saturated aqueous sodium chloride solution (5 x 50 mL), dried over sodium sulfate, filtered, and concentrated in vacuo. Silica gel chromatography (Gradient: 0percent to 50percent ethyl acetate in petroleum ether) afforded the product as a yellowsolid. Yield: 13 g, 48 mmol, 61percent. NMR (400 MHz, CDCI3) oe 9.94 (br s, 1 H), 8.65 (dd, J=4.5, 1.1 Hz, 1H), 7.78 (dd, J=8.4, 1.0 Hz, 1H), 7.31 (dd, J=8.4, 4.5 Hz, 1H), 4.49 (q, J=7.1 Hz, 2H), 1.45 (t, J=7.1 Hz, 3H). |
With pyridine; pyridinium hydrobromide perbromide; at 50℃; for 0.25h; | Ethyl 3-bromo-1H-pyrrolo[3,2-b]pyridine-2-carboxylate 0.9 g of pyridinium tribromide in 5 ml of pyridine is added slowly, at 0° C. under argon, to a solution of 0.5 g of <strong>[17288-32-3]ethyl 1H-pyrrolo[3,2-b]pyridine-2-carboxylate</strong> in 12 ml of pyridine. The solution is then heated at 50° C. for 15 min and then poured onto 100 ml of ice-cold water. The solid formed is filtered off, washed with water, and filter-dried. After drying under vacuum, 0.56 g of ethyl 3-bromo-1H-pyrrolo[3,2-b]pyridine-2-carboxylate are obtained, the characteristics of which are as follows: MS (ES+) spectrum: m/z=270 [MH]+ Melting point=180° C. (Koefler bench). IR spectrum (KBr): 2983; 2841; 2681; 1711; 1513; 1374; 1346; 1261 1209; 1012; 767 and 651 cm-1 |
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