Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1158953-95-7 | HCID 71755921 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 42629164 | HCID 42629164 | 87% |
Reaction Steps
156.9 g (2.4 mol) of zinc, 500 ml of ethanol and then 77 g (0.3 mol) of 4-fluoro-6-methyl-3-nitrobenzenesulfonyl chloride were placed in a 2-liter eggplant-shaped flask equipped with a mechanical stirrer, a thermometer and a dropping funnel. Thereinto was dropped 500 g (5 mol) of hydrochloric acid in a water bath so that the temperature of the reaction system did not exceed 50° C., followed by stirring at 75° C. for 6 hours. Ethanol was distilled off under reduced pressure; the residue was cooled to room temperature; sodium bicarbonate was added to neutralize the reaction system; extraction was conducted twice with ethyl acetate; the ethyl acetate layer was washed with water and then with a saturated aqueous sodium chloride solution. The ethyl acetate layer was dried with anhydrous sodium sulfate and subjected to distillation under reduced pressure to distil off ethyl acetate to obtain 41 g of a title compound at a yield of 87%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08334410B2 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-eae6ada18a4a46f7a3e05c2791ca5f85 |
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| Source note | uspto-grants-2012_12 |
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