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CAS No. : | 19520-75-3 | MDL No. : | MFCD06655980 |
Formula : | C8H8O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | TUUBOHWZSQXCSW-UHFFFAOYSA-N |
M.W : | 168.15 | Pubchem ID : | 7472024 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319 | 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 |
---|---|---|
98% | With sodium hydroxide In methanol at 45℃; Inert atmosphere | General procedure: To the solution of 3a (4.5 g, 16.7 mmol) in methanol (30 mL) was added 1 M sodium hydroxide (60 mL, 60 mmol), stirred at 45°C for 1-2 hours under nitrogen, monitored by TLC, followed by addition of 1 M hydrochloric acid (50 mL) to acidify the solution and extracted with ethyl acetate (3 × 50 mL). The combined organic layers was washed with distilled water (2 × 30 mL) and dried over sodium sulfate. The solvent was evaporated under reduced pressure to afford 5a as an off-white solid (4.02 g, 94percent), mp 196-198°C. 1H NMR (400 MHz, Acetone-d6) δ (ppm) 7.42-7.33 (5H, m, benzyl Ph), 7.21 (1H, dd, J=2.4, 1.2 Hz, H-2), 7.11 (1H, dd, J=2.4, 1.2 Hz, H-6), 6.68 (1H, t, J=2.4 Hz, H-4), 5.07 (2H, s, benzyl CH2). The 1H NMR spectrum was in good agreement with previously reported data[38]. |
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