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CAS No. : | 852054-42-3 | MDL No. : | MFCD08690306 |
Formula : | C7H5BrO3S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | YEKBJVHBVICUOZ-UHFFFAOYSA-N |
M.W : | 249.08 | Pubchem ID : | 11391008 |
Synonyms : |
|
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 |
---|---|---|
91% | With N-Bromosuccinimide; In acetonitrile; at 0 - 20℃; for 60h;Inert atmosphere; | Compound 1 (4.04 g, 23.7 mmol) was suspended in dry acetonitrile (100 mL) and cooled to0 C. NBS (4.36 g, 26.0 mmol), 1.1 equiv, was added and the mixture was stirred for 60 h atroom temperature, shielded from light and under nitrogen. The color changed from yellow topurple. The mixture was transferred with 150 mL of ethyl acetate to a separation funnel,washed with 10% aqueous Na2CO3 (2×200 mL), saturated Na2S2O3 (2×200 mL) and water(2×200 mL), dried with MgSO4, and evaporated in vacuo. Recrystallization twice from ethanol (60 mL) yielded 5.35 g (91%) of the bromide as yellow needles. 1H NMR (300 MHz,CDCl3 delta ppm ): 9.83 (s, 1H), 4.36 (m, 4H); 13C NMR (75 MHz, CDCl3 delta ppm):179.0, 147.9,140.4, 118.8, 102.0, 65.5, 65.1. |
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