Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 66583977 | HCID 66583977 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66584010 | HCID 66584010 | — |
Reaction Steps
7.7 ml of glacial acetic acid (0.135 moles) are added to a solution of 30 g of 2-nitro-5-(3-difluoromethoxyphenylthio)-p-xylene (0.092 moles) in H2O (40 ml) and ethanol (400 ml); 34.7 g of Fe in powder form (0.621 moles) are carefully added to the reaction mixture kept under stirring at 60° C. The temperature is brought to 90° C. and the mixture is kept under stirring for 1.5 hours. When the reaction is completed (GC and TLC analyses), the mixture is cooled to room temperature; the solid is filtered on a celite bed. The ethanol is concentrated at reduced pressure. The crude product obtained is washed with a saturated solution of sodium bicarbonate and extracted with ethyl acetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09040457B2 |
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| Source dataset | uspto-grants-2015_05 |
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| ORD ID | ord-de4f52406f1841e2bd2bcb353273031d |
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| Source note | uspto-grants-2015_05 |
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