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CAS No. : | 704-04-1 | MDL No. : | MFCD06409124 |
Formula : | C8H8FNO2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 169.15 | 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 |
---|---|---|
With trichlorophosphate In N,N-dimethyl-formamide | 64 Preparation 64 Preparation 64 At 5 °C was added phosphorus oxychloride (2.33ml) to N,N-dimethylformamide (15ml). Stirred 30 minutes at 5 °C under nitrogen and added 5-fluoro-2-methoxybenzamide (1.40g). Stirred 1 hour at 5°C. Poured into water (100ml), allowed to stand for 30 minutes, collected by filtration, washed with water, and air dried to give 5-fluoro-2-methoxybenzonitrile (1.45g) as white crystals. mp:113-114°C IR(KBr):2229cm-1 MS:152(M+1) NMR(DMSO, δ):3.90(3H,s), 7.27(1H,dd,J=9.4Hz,4.2Hz), 7.58(1H,ddd,J=9.2Hz, 9.2Hz,3.2Hz), 7.75(1H,dd,J=8.2Hz,3.2Hz) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium methylate In N,N-dimethyl-formamide | 65 Preparation 65 Preparation 65 A solution of methyl 5-fluoro-2-methoxybenzoate (2.20g), N,N-dimethylformamide (10ml), and sodium methoxide (100mg) was heated at 100°C for 7 hours. Cooled to room temperature, diluted with ethyl acetate (100ml), washed with water (three times, 100ml each time), brine (100ml), dried over Magnesium sulfate, filtered, evaporated, and purified by silica gel column chromatography (dichloromethane/methanol) to give 5-fluoro-2-methoxybenzamide (1.48g) as white crystals. mp:144-146°C IR(KBr):3448,1674cm-1 MS:170(M+1) NMR(DMSO, δ):3.88(3H,s), 7.16(1H,dd,J=9.1Hz,4.4Hz), 7.33(1H,ddd,J=9.1Hz, 9.1Hz,3.4Hz), 7.53(1H,dd,J=9.4Hz,3.3Hz), 7.70(2H,s) |