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CAS No. : | 604000-97-7 | MDL No. : | MFCD12026481 |
Formula : | C8H5FO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | MBTIUAFUJPATDP-UHFFFAOYSA-N |
M.W : | 168.12 | Pubchem ID : | 18441958 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302 | 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% | Stage #1: With sodium hydride In N,N-dimethyl-formamide at 0 - 20℃; Stage #2: for 2 h; |
Sodium hydride (69 mg, 1.7 mmol) was added portionwise to a solution of 2-fluoro-4- formylbenzoic acid (0.30 g, 1.4 mmol) in N,N-Dimethylformamide (5.0 mL) at 0 °C. The mixture was allowed to warm to room temperature and was stirred for 30 minutes. Methyl iodide (0.18 mL, 2.9 mmol) was introduced dropwise. After 2 hours, the mixture was quenched with 1 N HC1, and extracted with EtOAc. The extracts were washed with water (twice), brine (once), dried over sodium sulfate and concentrated. Flash columnchromatography, eluting with a gradient from 0- 15percent ethyl acetate in hexanes afforded product as a white solid (190 mg, 72percent).3/4 NMR (300 MHz, CDC13): δ 10.05 (d, 1H), 8.11 (dd, 1H), 7.73 (dd, 1H), 7.65 (dd, 1H), 3.98 (s, 3H); LCMS (M+H)+: 183.0. |
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