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CAS No. : | 121-92-6 | MDL No. : | MFCD00007251 |
Formula : | C7H5NO4 | Boiling Point : | No data available |
Linear Structure Formula : | (O2N)C6H4COOH | InChI Key : | AFPHTEQTJZKQAQ-UHFFFAOYSA-N |
M.W : | 167.12 | Pubchem ID : | 8497 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P273-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335-H412 | 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 |
---|---|---|
76% | With pyridine; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; at 20℃; for 3h;Inert atmosphere; | To the suspension of 3-nitrobenzoic acid ( 1 g, 5.98 mmol) in pyridine ( 10ml) <strong>[42303-42-4]ethyl <strong>[42303-42-4]1-aminocyclopropanecarboxylate hydrochloride</strong></strong> ( 1.090 g, 6.58 mmol) was added followed by EDC.HC1 (1.721 g, 8.98 mmol) under nitrogen. Reaction mixture was stirred at room temperature for 3hrs. Reaction mixture was diluted with cold water ( 100ml) and extracted with ethyl acetate (2X25ml). Separated organic layer was washed with brine and water, dried over sodium sulfate and concentrated under vacuum till dryness to obtain product ( 1.26g, 76%). NMR (400 MHz, CDC13) 8 (ppm): 8.59 (bs, 1H), 8.41-8.38 (m, 1H), 8.20-8. 18(m, 1H), 7.68 (t, 1H, J=8Hz), 6.82 (bs, 1H), 4.19 (q, 2H, J=7.2Hz), 1.70- 1.34 (m, 2H), 1.37- 1.33 (m, 2H), 1.26(t,3H,J=7.2Hz). ESI- MS (m/z): 279.58 (M+l) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
240 mg | With pyridine; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; at 22 - 26℃; for 10h;Inert atmosphere; | Step-a: Synthesis of 3-Nitro-N-(tetrahydrofuran-3-yl)benzamide Tetrahydrofuran-3-amine (0.1 g, 1.148 mmol) and 3-nitrobenzoic acid (0.192 g, 1.148 mmol) were taken in pyridine (2 ml), to the mixture EDC.HCl (0.220 g, 1.148 mmol) was added, the reaction mixture was stirred under nitrogen for 10 hrs at room temperature. The reaction mixture was diluted with cold water (15 ml), extracted with ethyl acetate (2*10 ml). Combined organic layer was washed with satd. aq. sod bicarbonate and dil HCl, the organic layer was dried over sodium sulfate and concentrated under vacuum to afford the title product (240 mg). 1HNMR (400 MHz, CDCl3): delta 8.62-8.61 (m, 1H), 8.39-8.36 (m, 1H), 8.19-8.17 (m, 1H), 7.67 (t, 1H, J=8 Hz), 6.62 (d, 1H, J=6 Hz), 4.79-4.75 (m, 1H), 4.08-4.00 (m, 1H), 3.93-3.83 (m, 3H), 2.44-2.37 (m, 1H), 2.01-1.98 (m, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
76% | With pyridine; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; at 22 - 26℃; for 3h;Inert atmosphere; | Step-a: Synthesis of Ethyl 1-(3-nitrobenzamido)cyclopropanecarboxylate To the suspension of 3-nitrobenzoic acid (1 g, 5.98 mmol) in pyridine (10 ml) <strong>[42303-42-4]ethyl <strong>[42303-42-4]1-aminocyclopropanecarboxylate hydrochloride</strong></strong> (1.090 g, 6.58 mmol) was added followed by EDC.HCl (1.721 g, 8.98 mmol) under nitrogen. Reaction mixture was stirred at room temperature for 3 hrs. Reaction mixture was diluted with cold water (100 ml) and extracted with ethyl acetate (2*25 ml). Separated organic layer was washed with brine and water, dried over sodium sulfate and concentrated under vacuum till dryness to obtain product (1.26 g, 76%). 1H NMR (400 MHz, CDCl3) delta (ppm): 8.59 (bs, 1H), 8.41-8.38 (m, 1H), 8.20-8.18 (m, 1H), 7.68 (t, 1H, J=8 Hz), 6.82 (bs, 1H), 4.19 (q, 2H, J=7.2 Hz), 1.70-1.34 (m, 2H), 1.37-1.33 (m, 2H), 1.26 (t, 3H, J=7.2 Hz). ESI-MS (m/z): 279.58 (M+1) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77.1% | With dmap; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In dichloromethane; at 2 - 20℃; for 2.25h; | 7-Et-CPT (0.75?g, 2?mmol), EDCI (1.53g, 8?mmol) and DMAP (1.47?g, 12?mmol) were added to a solution of m-nitrobenzoic acid (1.00?g, 6?mmol) in 100?mL of CH2Cl2 with stirring at 2?°C for 15?min. The mixture was stirred at room temperature for 2?h and was poured onto 100?ml ice water. The obtained organic layer was washed with dilute hydrochloric acid and saturated salt water in turn, and concentrated. The crude product was chromatographically separated with CH2Cl2-THF as eluent. The pure product 3g (0.81?g) was obtained as almost white powder, yield 77.1percent, purity 98.97percent (HPLC), mp 272-274?°C. 1H NMR (CDCl3, 500?MHz) delta: 1.11 (t, J?=?7.5?Hz, 3H, 19-H), 1.40 (t, J?=?7.8?Hz, 3H, 30-H), 2.37-2.49 (m, 2H, 18-H), 3.20 (q, 2H, 29-H), 5.25 (d, J?=?18.5?Hz, 1H, 5-H), 5.29 (d, J?=?19.0?Hz, 1H, 5-H), 5.49 (d, J?=?17.0?Hz, 1H, 17-H), 5.79 (d, J?=?17.0?Hz, 1H, 17-H), 7.25 (s, 1H, 14-H), 7.68 (m, 2H, 10, 27-H), 7.77 (t, J?=?7.5?Hz, 1H, 11-H), 8.13 (t, J?=?9.8?Hz, 2H, 9,12-H), 8.40 (d, J?=?7.5?Hz, 1H, 24-H), 8.46 (m, 1H, 26-H), 8.93 (s, 1H, 28-H). ESI-MS m/z: 526.2 (M?+?1)+. |
[ 3807-81-6 ]
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