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CAS No. : | 62726-03-8 | MDL No. : | MFCD12913504 |
Formula : | C8H8N2O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 196.16 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* 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 |
---|---|---|
95% | With ammonium hydroxide In methanol for 10h; Ambient temperature; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
74% | With pyridine; ammonium chloride; 2,4,6-tripropyl-1,3,5,2,4,6-trioxatriphosphinane-2,4,6-trioxide In ethyl acetate at 60℃; for 18h; | 1.5.A 2-Methoxy-4-nitrobenzamide 2-Methoxy-4-nitrobenzamide 1.50 g (7.61 mmol) of 2-methoxy-4-nitrobenzoic acid and 1.22 g (22.83 mmol, 3 eq.) of ammonium chloride were initially charged in 26 ml of pyridine and heated to 60° C., 7.23 ml (30.43 mmol, 50% in ethyl acetate, 4.0 eq.) of T3P were added and the mixture was stirred at 60° C. for 18 h. The reaction mixture was cooled down and admixed with 100 ml of ethyl acetate and 30 ml of saturated aqueous sodium hydrogencarbonate solution. Subsequently, ethyl acetate and pyridine were removed on a rotary evaporator. The aqueous suspension was filtered and the remaining solids were washed with water, isopropanol and then pentane, and dried. Yield: 1.15 g (74% of theory). LC/MS [Method 1]: Rt=0.56 min; MS (ESIpos): m/z=197 (M+H)+, 1H-NMR (400 MHz, DMSO-d6): δ [ppm]=7.90-7.84 (m, 3H), 7.80 (s, 1H), 7.76 (s, 1H), 3.98 (s, H). |
Multi-step reaction with 2 steps 1: oxalyl dichloride; N,N-dimethyl-formamide / dichloromethane / 1 h / 20 °C / Inert atmosphere 2: ammonium hydroxide / dichloromethane / Inert atmosphere |