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CAS No. : | 21928-51-8 | MDL No. : | MFCD00155009 |
Formula : | C6H2BrCl3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | VZUMVBQMJFFYRM-UHFFFAOYSA-N |
M.W : | 260.34 | Pubchem ID : | 4124400 |
Synonyms : |
|
Chemical Name : | 5-Bromo-1,2,3-trichlorobenzene |
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 |
---|---|---|
99% | In an oven dried, nitrogen flushed, 500 mL round-bottomed flask equipped with a pressure equalizing addition funnel, 5-bromo- 1,2,3-trichlorobenzene ( 10.0 g, 38.4 mmol) was dissolved in tetrahydrofuran ( 100 mL), and the resulting solution was cooled in an ice bath under nitrogen. /soPropyl magnesium chloride (2 M solution tetrahydrofuran, 21. 1 mL, 42.3 mmol) was added dropwise with good stirring over 15 minutes via the addition funnel . After 0.5 hours, Lambda/,N-dimethylformamide (3.72 mL, 48.0 mmol) was added to the dark solution with stirring . After an additional 0.5 hours, hydrochloric acid ( 1 N, 100 mL) was added with stirring . The layers were separated, and the organic layer was washed with brine. The combined aqueous layers were extracted with ether, and the combined organics were dried over sodium sulfate, filtered, and concentrated to afford the title compound as a white solid ( 10 : 1 mixture of title compound to 1,2,3-trichlorobenzene, 7.96 g, 99%) : NM R (CDCb) delta 9.91 (s, 1H), 7.88 (s, 2H) ; EIMS m/z 209 ( [M ]+). | |
99% | Example 56 Preparation of 3,4,5-trichlorobenzaldehyde (C96) In an oven dried, nitrogen flushed, 500 mL round-bottomed flask equipped with a pressure equalizing addition funnel, 5-bromo-1,2,3-trichlorobenzene (10.0 g, 38.4 mmol) was dissolved in tetrahydrofuran (100 mL), and the resulting solution was cooled in an ice bath under nitrogen. isoPropyl magnesium chloride (2 M solution tetrahydrofuran, 21.1 mL, 42.3 mmol) was added dropwise with good stirring over 15 minutes via the addition funnel. After 0.5 hours, N,N-dimethylformamide (3.72 mL, 48.0 mmol) was added to the dark solution with stirring. After an additional 0.5 hours, hydrochloric acid (1 N, 100 mL) was added with stirring. The layers were separated, and the organic layer was washed with brine. The combined aqueous layers were extracted with ether, and the combined organics were dried over sodium sulfate, filtered, and concentrated to afford the title compound as a white solid (10:1 mixture of title compound to 1,2,3-trichlorobenzene, 7.96 g, 99%): 1H NMR (CDCl3) delta 9.91 (s, 1H), 7.88 (s, 2H); EIMS m/z 209 ([M]+). |
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