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CAS No. : | 72517-15-8 | MDL No. : | MFCD08669420 |
Formula : | C7H5BrO4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | KUVLHMSXBCGHEY-UHFFFAOYSA-N |
M.W : | 233.02 | Pubchem ID : | 12394883 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-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 |
---|---|---|
78% | Stage #1: at 20℃; for 0.5 h; Stage #2: at 20℃; for 9 h; Heating / reflux |
A mixture of thionyl chloride (0.35 mL, 4.8 mmol) and methanol (5.4 mL) was stirred at room temperature for 30 min then treated with part B compound (600 mg, 2.57 mmol). The reaction mixture was stirred at room temperature for 2.0 hr. refluxed for 7.0 hr, cooled and concentrated to a brown solid. Purification by column chromatography (2.5.x.25 cm column, 1:4 EtOAc/hexane, then 1:1 EtOAc) gave the title compound (500 mg, 78percent). |
12.5 g | at 0℃; Reflux; Inert atmosphere | SOCl2(13.1 mL, 180.9 mmol) was added dropwise into a solution of the compound (17-1) (14.1 g, 60.3 mmol) in 27 MeOH (200 mL) at 0°C in a nitrogen atmosphere. A resulting mixture was stirred at reflux overnight. After a reaction was completed, a volatile solvent was evaporated under reduced pressure. A resulting residue was purified by means of a silica gel column chromatography, so as to obtain the 106 title compound (17-2) (12.5 g, 50.6 mmol, 84percent). (0144) 1H NMR (400 MHz, CDCl3); δ 10.85 (s, 1H), 7.51 (s, 1H), 7.23 (s, 1H), 5.69 (s, 1H), 3.96 (s, 3H) |