* Storage: Keep in dark place,Inert atmosphere,Store in freezer, under -20°C
* Shipping: Normal
CAS No. : | 690635-35-9 | MDL No. : | MFCD14581634 |
Formula : | C8H8ClN3O4 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 245.62 | Pubchem ID : | - |
Synonyms : |
Signal Word: | Warning | Class: | |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302 | 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 |
---|---|---|
52.6% | With ammonia; In 1,4-dioxane; dichloromethane; at 0 - 20℃; for 24h; | Step 4: Preparation of ethyl 4-amino-6-chloro-5-nitronicotinate (17) To a solution of <strong>[154012-15-4]ethyl 4,6-dichloro-5-nitronicotinate</strong> 16 (15.0 g, 56.6 mmol) in dichloromethane 85 ml was added saturated ammonia solution in 1,4-dioxane 115 ml at 0 C. The resulting mixture was then stirred at ambient temperature for 24 h. Solvent was removed under reduced pressure and the residue was subjected to silica gel column chromatography using ether/ethyl acetate (15:1) as eluent to give 17 7.3 g as yellow crystalline solid, yield 52.6%. Mp 118-120 C. 1H NMR (300 MHz, DMSO-d6), delta (ppm): 8.62 (s, 1H), 8.05 (br s, 2H), 4.33 (q, J = 6.0 Hz, 2H), 1.31 (t, J = 6.0 Hz, 3H). MS (ESI(+) 70 V) m/z: 246 [M+H]+. |
With ammonia; triethylamine; In 1,4-dioxane; dichloromethane; at 0℃; | To a solution of 4,6-Dichloro-2-methyl-5-nitro-pyridine-3-carboxylic acid (15 g, 56.6 mmol) and triethylamine (7.9 ML, 57.3 mmol) in dichloromethane (84 ML) at 0 C. was added dropwise ammonia solution in dioxane (0.5 M, 113 ML, 56.5 mmol).The mixture was then stirred overnight.Removal of the solvent followed by column chromatography gave 9 as a yellow crystalline solid. (7.3 g).1H-NMR delta: 1.32 (t, J=7.1 Hz, 3H), 4.33 (q, J=7.1 Hz, 2H), 8.06 (s, br, 2H), 8.62 (s, 1H). |