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CAS No. : | 13162-27-1 | MDL No. : | MFCD08062586 |
Formula : | C5H5Cl2N3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | FDMMHWIFYCXEOF-UHFFFAOYSA-N |
M.W : | 178.02 | Pubchem ID : | 14665971 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H317-H319 | 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 |
---|---|---|
74.4% | With palladium on activated charcoal; hydrogen; triethylamine In ethanol; water for 8 h; | The raw material 14 (2.63g), adding 263mg of Pd / C, adding triethylamine 3.5ml, anhydrous ethanol 88ml, water 4ml, 20psi hydrogen pressure reaction 8h, the raw material reaction is complete after the filter, spin dry solvent, Yellow solid, dry loading, purification to obtain white solid 15 (1.22g) yield 74.4percent. |
20% | With hydrogen; magnesium oxide In ethanol; water at 20℃; | Example 31; 2-[4-(4-chloro-benzyl)-5-methyl-4H-[1,2,4]triazol-3-yl]-pyrrolidine-1-carboxylic acid (2-chloro-4-methyl-pyrimidin-5-yl)-amide; Step A; 2,4-Dichloro-6-methylpyrimidin-5-amine (1.0 g, 5.62 mmol) was dissolved in anhydrous EtOH (3.5 mL) and H2O (7.0 mL). MgO (1.40 g, 34.74 mmol) and 10percent Pd/C (35 mg) were added to the reaction mixture which was hydrogenated at 1 atm, at room temperature, overnight. The reaction mixture was filtered and concentrated. The residue was purified by silica gel column chromatography (MeOH/CH2Cl2 gradient, 0-15percent MeOH) to afford 2-chloro-4-methylpyrimidin-5-amine as light pink solid (0.16 g, 20percent).1H NMR (300 MHz, CD3OD) 2.36 (s, 3H), 7.95 (s, 1H). MS: calculated: 143.03, found (MH+): 144.0. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65.1% | With palladium on activated charcoal; hydrogen In ethyl acetate at 20℃; | The raw material 13 (860mg) and Pd / C (180mg) were dissolved in ethyl acetate (30ml), hydrogen was ventilated three times, reacted at room temperature under hydrogen pressure 40psi. After the reaction was complete, Pd / C was filtered, To give a yellow solid 14 (500 mg) in 65.1percent yield. |
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