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CAS No. : | 824-42-0 | MDL No. : | MFCD00040798 |
Formula : | C8H8O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IPPQNXSAJZOTJZ-UHFFFAOYSA-N |
M.W : | 136.15 | Pubchem ID : | 522777 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | 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 |
---|---|---|
95% | With bromine; acetic acid; at 0℃; for 2h; | The compound BB-8-1 (5g, 36.72mmol) was dissolved in acetic acid (30mL), cooled to 0 , then added dropwise liquid bromine(6.75g, 42.23mmol), which was allowed to react at 0 2 hours.After completion of the reaction, water was added (100 mL), filtered, solid waswashed with water, and dried to give the title compound BB-8-2 (yellow solid, 7.5g, yield: 95%) |
89% | With bromine; acetic acid; at 20℃; for 2h;Cooling with ice; | Under an ice bath, bromine (4.6 g, 28.75 mmol) was added to a solution of 2-hydroxy-3-methylbenzaldehyde (3.4 g, 25.0 mmol) in glacial acetic acid (20 mL), and the reaction solution was stirred at room temperature for 2 h. Water (100 mL) was added to the reaction solution, and the precipitated solid was filtered out. The filter cake was washed with water (100 mL) and dried under vacuum to give 5-bromo-2-hydroxy-3-methylbenzaldehyde (4.8 g, 89%) in the form of a yellow solid, which was directly used in the next step. LCMS (ESI) [M+H]+=216.9; 1H NMR (400 MHz, CDCl3) δ 11.19 (s, 1H), 9.82 (s, 1H), 7.66-7.46 (m, 2H), 2.26 (s, 3H). |
88.6% | With bromine; In acetic acid; at 0℃; for 2h; | [1050] The solution of 2-Hydroxy-3-methylbenzaldehyde (1.0 g, 7.35 mmole) in acetic acid (6 mL) was cooled to 0 C (ice bath). Bromine (1.36 g, 8.52 mmole) was added dropwise and allowed to stir for 2 hours. The reaction was warmed to room temperature and diluted with water (100 mL) yielding a light orange precipitate. The solid was filtered and washed with water (10 mL). Dried on high vacuum to give a light brown solid (1.4 g, 88. 6%). 1H NMR (CDC13/400 MHz) 11.16 (s, 1H), 9.79 (s, 1H), 7.48 (s, 1H), 7.46 (s, 1H), 2.23 (s, 3H). |
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