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CAS No. : | 17288-52-7 | MDL No. : | MFCD08437635 |
Formula : | C8H6N2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | DQSXESUAVDEVJI-UHFFFAOYSA-N |
M.W : | 146.15 | Pubchem ID : | 22281739 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302 | 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 |
---|---|---|
90% | With manganese(IV) oxide; In tetrahydrofuran; at 20℃; for 18.0h; | General procedure: [0078] To a solution of (5-(trifluoromethyl)-1H-indol-2-yl)methanol (751 mg,3.49 mmol) in THF (25 mL) was added MnCfi (3034 mg,34.9 mmol) and the mixture was stirred at room temperature for 18 hours. The mixture was then diluted with ethyl acetate and filtered through a pad of celite to afford 5-(trifluoromethyl)-1H-indole-2-carbaldehyde as a yellow solid. [0079] Yield 541 mg (73%, over 2 steps). 1H NMR (400 MHz, DMSO) d 12.40 (s, 1H), 9.95 (s, 1H), 8.23 (s, 1H), 7.66 (d, J=8.9 Hz, 1H), 7.62 (dd, J=1.5, 8.9 Hz, 1H), 7.58 (d, J=1.5 Hz, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
(a) 1H-Pyrrolo[3,2-b]pyridin-2-carboxaldehyde This was prepared from methyl 1H-pyrrolo[3,2-b]pyridin-2-carboxylate (0.1 g) and amine (1d) by the method of Example 16c, (except that the alcohol was stirred with manganese (II) oxide overnight) and used without purification. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48.9% | With water monomer; sodium hydroxide; In tetrahydrofuran; methanol; at 0 - 20℃; for 1.0h; | 1-(Phenylsulfonyl)-1H-pyrrolo[3,2-b]pyridine-2-carbaldehyde (1.2 g, 4.1 mmol, 1.0 eq) was dissolved in anhydrous THF (15 mL).Cool down to 0 C,A methanol/water mixed solution (1:1 v/v, 30 mL) of sodium hydroxide (1.67 g, 41 mmol, 10 eq) was added dropwise.After the completion of the dropwise addition, the mixture was slowly returned to room temperature for 1 hour.The reaction was completely confirmed by LC-MS and TLC, and the mixture was stirred and evaporated to ethylamine (20mL).The organic phases are combined, washed with saline, dried and concentrated.The crude product was purified by silica gel column chromatography to yield yellow solidThe product was obtained (300 mg, yield: 48.9%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
42.8% | With potassium carbonate; In N,N-dimethyl-formamide; at 40℃; for 2.0h; | 1H-Pyrolo[3,2-b]pyridine-2-carbaldehyde (294 mg, 2 mmol, 1.0 eq) was dissolved in dry DMF (5 mL)Potassium carbonate (552.8 mg, 4 mmol, 2.0 eq) and ethyl iodide (375 mg, 2.4 mmol, 1.2 eq) were added, and the mixture was heated to 40 C for 2 hours. The reaction was completed by LC-MS and TLC, poured into ice water (10 mL), extracted with EA (20 mL×2), washed with brine, dried and concentrated.The product was obtained (150 mg, yield: 42.8%). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
64% | With piperidine; In ethanol; for 4.0h;Reflux; | General procedure: A mixture of 2a-2n (0.38 mmol), aldehyde 3a-3p and 44 (or ketone 39-43) (0.42 mmol) and piperidine (37.5 μL, 0.38 mmol) in ethanol (3.0 mL) was refluxed for the given time as described individually. The reaction was monitored by TLC. The purification was performed in either of the following two methods. Purification 1. When the product is crystalized as solid during reaction, the reaction mixture was cooled to room temperature slowly. The precipitate is collected by using vacuum filtration with washing cold EtOH. The collected product was dried under low pressured vacuum to give a desired product. |
64% | With piperidine; In ethanol; for 4.0h;Reflux; | General procedure: A mixture of 2a-2n (0.38 mmol), aldehyde 3a-3p and 44 (or ketone 39-43) (0.42 mmol) and piperidine (37.5 μL, 0.38 mmol) in ethanol (3.0 mL) was refluxed for the given time as described individually. The reaction was monitored by TLC. The purification was performed in either of the following two methods. Purification 1. When the product is crystalized as solid during reaction, the reaction mixture was cooled to room temperature slowly. The precipitate is collected by using vacuum filtration with washing cold EtOH. The collected product was dried under low pressured vacuum to give a desired product. |
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