Purity | Size | Price | VIP Price | USA Stock *0-1 Day | Global Stock *5-7 Days | Quantity | ||||||
{[ item.p_purity ]} | {[ item.pr_size ]} | Inquiry |
{[ getRatePrice(item.pr_usd, 1,1,item.pr_is_large_size_no_price) ]} {[ getRatePrice(item.pr_usd,item.pr_rate,1,item.pr_is_large_size_no_price) ]} |
{[ getRatePrice(item.pr_usd, 1,1,item.pr_is_large_size_no_price) ]} | Inquiry {[ getRatePrice(item.pr_usd,item.pr_rate,item.mem_rate,item.pr_is_large_size_no_price) ]} {[ getRatePrice(item.pr_usd,1,item.mem_rate,item.pr_is_large_size_no_price) ]} | {[ item.pr_usastock ]} | in stock Inquiry - | {[ item.pr_chinastock ]} | {[ item.pr_remark ]} in stock Inquiry - | Login | Inquiry |
Please Login or Create an Account to: See VIP prices and availability
CAS No. : | 6317-97-1 | MDL No. : | MFCD01765414 |
Formula : | C8H8N2O6 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | JBTWWCUXSHUDEJ-UHFFFAOYSA-N |
M.W : | 228.16 | Pubchem ID : | 54694073 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | 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 |
---|---|---|
72% | I] Preparation of compound 5-1 2.0 g (8.77 mmol) of compound 5-H in 8.0 ml (86 mmol) phosphorus oxychloride are stirred at 800C for 74 hours. About half of the phosphorus oxychloride is then removed in vacuo and the remainig mixture is poured onto ice. The mixture is extracted with 3 x 30 ml of ethyl acetate. The combined organic phases are washed with 30 ml of aqueous sodium carbonate (10%), 2 x 30 ml water and 30 ml of brine, dried over Na2SO4 and evaporated in vacuo to give the crude product as a brown oil which is purified by column chromatography on silica gel (ethyl acetate/hexane 1:20) to give 1.67 g (72%) of the desired product as light yellow solid.1H-NMR (DMSO-de): 9.08 (s, IH); 4.40 (q, 2H); 1.35 (t, 3H). | |
72% | With trichlorophosphate; at 80℃; for 74h; | 2.0 g (8.77 mmol) of the product of example 8 step B in 8.0 ml (86 mmol) phosphorus oxychloride were stirred at 8O0C for 74 hours. About half of the phosphorus oxychloride was then removed in vacuo and the remainig mixture was poured onto ice. The mixture was extracted with 3 x 30 ml of ethyl acetate. The combined organic phases were washed with 30 ml of aqueous sodium carbonate (10%), 2 x 30 ml water and 30 ml of brine, dried over Na2SO4 and evaporated in vacuo to give the crude product as a brown oil which was purified by column chromatography on silica gel (ethyl acetate/hexane 1:20) to give 1.67 g(72%) of the desired product as light yellow solid.1H-NMR (DMSOd6): 9.08 (s, IH); 4.40 (q, 2H); 1.35 (t, 3H). |
61.1% | With trichlorophosphate; at 80℃; for 24h; | Step 3: Preparation of ethyl 4,6-dichloro-5-nitronicotinate (16) A solution of ethyl 4,6-dihydroxy-5-nitronicotinate 15 (20.0 g, 87.7 mmol) in phosphorus oxychloride (80 ml, 874 mmol) was stirred at 80 C for 24 h. After half of the phosphorus oxychloride was removed under reduced pressure, the residue was poured into ice-water. The mixture was extracted with ethyl acetate twice, the combined organic phases were washed with aqueous sodium carbonate, water and brine respectively, dried over anhydrous Na2SO4. Filtration and evaporation gave the crude product as brown oil which was further purified by silica gel column chromatography using petroleum ether/ethyl acetate (3:1) as eluent to give 16 14.2 g as white crystalline solid, yield 61.1%. Mp 36-38 C. 1H NMR (300 MHz, DMSO-d6), delta (ppm): 9.07 (s, 1H), 4.39 (q, J = 6.0 Hz, 2H), 1.34 (t, J = 6.0 Hz, 3H). MS (ESI(+) 70 V) m/z: 264 [M+H]+. |
[ 6635-31-0 ]
6-Hydroxy-5-nitronicotinic acid
Similarity: 0.80
[ 89282-12-2 ]
4-Hydroxy-3-nitropyridin-2(1H)-one
Similarity: 0.75
[ 79398-27-9 ]
Methyl 4,6-dihydroxynicotinate
Similarity: 0.71
[ 6854-07-5 ]
5-Nitro-2-oxo-3-pyridinecarboxylic Acid
Similarity: 0.66
[ 79398-27-9 ]
Methyl 4,6-dihydroxynicotinate
Similarity: 0.71
[ 59237-50-2 ]
Methyl 5-amino-6-methoxynicotinate
Similarity: 0.69
[ 88312-64-5 ]
Methyl 2-amino-5-nitronicotinate
Similarity: 0.69
[ 271261-71-3 ]
Methyl 2,4-dihydroxy-5-nitrobenzoate
Similarity: 0.68
[ 6635-31-0 ]
6-Hydroxy-5-nitronicotinic acid
Similarity: 0.80
[ 89282-12-2 ]
4-Hydroxy-3-nitropyridin-2(1H)-one
Similarity: 0.75
[ 160590-36-3 ]
2-Methoxy-3-nitro-4-methylpyridine
Similarity: 0.69
[ 88312-64-5 ]
Methyl 2-amino-5-nitronicotinate
Similarity: 0.69
[ 2047-49-6 ]
5-Nitropyridin-3-ylcarboxylic acid
Similarity: 0.68
[ 6635-31-0 ]
6-Hydroxy-5-nitronicotinic acid
Similarity: 0.80
[ 89282-12-2 ]
4-Hydroxy-3-nitropyridin-2(1H)-one
Similarity: 0.75
[ 79398-27-9 ]
Methyl 4,6-dihydroxynicotinate
Similarity: 0.71
[ 59237-50-2 ]
Methyl 5-amino-6-methoxynicotinate
Similarity: 0.69