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CAS No. : | 36075-35-1 | MDL No. : | MFCD23703400 |
Formula : | C8H7N3O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MUMFMRMWLWUMDW-UHFFFAOYSA-N |
M.W : | 177.16 | Pubchem ID : | 23249447 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P301+P312-P302+P352-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H320-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 |
---|---|---|
92% | With 1,5-diazabicyclo[4.3.0]non-5-ene 2,2,2-trifluoroethanol; at 60.0℃; for 3.0h; | Compound 1b (1 mmol, 133 mg), [HDBN+][TFE-] (6 mmol, 1.35 g) was added to a 10 ml round bottom flask. In a CO2 environment, the reaction is heated to 60C for 3 hours, and the reaction is stopped. After the temperature is cooled to room temperature, a saturated aqueous NH4Cl solution is added. Adjust the pH to neutral, extract three times with 20ml CH2Cl2, collect the CH2Cl2 solution and dry it over anhydrous sodium sulfate. After filtration, the solution was removed by evaporation under reduced pressure, and the resulting solid was separated by silica gel column chromatography (eluent: CH2Cl2:CH3OH=15:1).163 mg of white solid compound 2b, yield 92%. |
92% | With 1,5-diazabicyclo[4.3.0]non-5-ene 2,2,2-trifluoroethanol; at 60.0℃; under 760.051 Torr; for 3.0h;Green chemistry; | General procedure: Substrate (1.0 mmol), [HDBN+][TFE-] (6.0 mmol) were loaded in a 10 mL glass reaction tube equipped with a magnetic stirrer. The air in the reactor was replaced by CO2. Then, the reactor was stirred at the desired temperature for 3-96 h under CO2 using a balloon. After the reaction, the reaction liquid was cooled to room temperature and quenched by saturated ammonium chloride solution. Then the mixture was filtered to afford the crude product, which was purified by chromatography (silica gel, methanol/dichloromethane=1/20) to give the desired compound. The purified product was characterized by NMR and HR-MS. 1H NMR and 13C NMR studies were carried out with a JEOL NMR 400 (400 MHz, 100 MHz) spectrometer with DMSO-d6 as the solvent. Mass spectra were recorded with an AMD40223(Interambulacra) spectrometer. |
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