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CAS No. : | 70593-57-6 | MDL No. : | MFCD01646073 |
Formula : | C6H4Cl2N2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IQVYHPUXNYVYFW-UHFFFAOYSA-N |
M.W : | 191.02 | Pubchem ID : | 600044 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-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 |
---|---|---|
73% | With sodium hydroxide; water; bromine; In 1,4-dioxane; at 0 - 25℃; for 18h; | NaOH (6.60 g, 165 mmol) was dissolved in H2O (31 mL) and cooled in an ice bath. Bromine (2.08 mL, 40.6 mmol) was added dropwise and the yellow solution was stirred for 15 min. 4,6-Dichloro-nicotinamide (7.27 g, 38.1 mmol) in 1,4-dioxane (21 mL) was added dropwise to the bromine solution over 30 min. The reaction was allowed to warm slowly to 25° C. over 18 h. The volatiles were removed in vacuo and the resultant solution was diluted with brine and poured into EtOAc. The aqueous phase was separated and extracted twice with EtOAc. The organic layers were combined, dried (Na2SO4), decanted and concentrated to afford an orange oil. The resultant oil was purified on a 100 g SiO2 flash chromatography cartridge with 25 percent EtOAc-hexanes to afford 4,6-dichloro-pyridin-3-ylamine as a tan solid (4.54 g, 73percent). 30percent Aqueous H2O2 solution (29 mL) was cooled in an ice bath. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N-ethyl-N,N-diisopropylamine; In ethanol; N,N-dimethyl acetamide; at 60℃; | Example 137; Synthesis of 2-[4-(quinolin-3-yl)-9H-carbazol-9-yl]-4-(tetrahydropyran-4-yl)amino)pyridine-5-carboxamide; Stage 1:; In a 25 ml single-necked round-bottomed flask, 300 mg of 4,6-dichloronicotinamide are dissolved in 4.5 ml of ethanol and 4.5 ml of dimethylacetamide, and then 238 mg of 4-aminotetrahydropyran hydrochloride and 711 mg of diisopropylethylamine are added. The mixture is then heated overnight at 60° C. After concentration under reduced pressure, the residue is extracted with dichloromethane, washed with water, dried over magnesium sulphate and concentrated under reduced pressure. After purification by flash chromatography on 25 g of silica, elution being carried out with a mixture of ethyl acetate and heptane (85/15 by volume), 132.5 mg of 6-chloro-4-(tetrahydropyran-4-yl)aminonicotinamide are obtained, the characteristic of which is the following: 1H NMR spectrum (400 MHz, DMSO-d6, delta ppm): 1.32-1.46 (m, 2 H) 1.88 (d, J=11.2 Hz, 2 H) 3.47 (td, J=11.2, 2.2 Hz, 2 H) 3.66-3.77 (m, 1 H) 3.82 (dt, J=11.7, 3.6 Hz, 2 H) 6.82 (s, 1 H) 7.45 (broad s, 1 H) 8.07 (broad s, 1 H) 8.41 (s, 1 H) 8.86 (d, J=8.1 Hz, 1 H). |
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