Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Tin tetrachloride | HCID 24287 | — |
| Reactant | HCID 71084709 | HCID 71084709 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 89260527 | HCID 89260527 | 61% |
Reaction Steps
1-(4-Chloro-3-(trifluoromethyl)phenyl)-3-(4-methyl-3-nitrophenyl)urea (7 g, 18.7 mmol) obtained in Step (1) above was stirred in a solvent of ethanol (100 mL). The reaction solution was added with tin chloride (II) dihydrate (12.68 g, 56.2 mmol), followed by stirring for about 4 hours at 80° C. The reaction mixture was diluted with ethyl acetate, and washed with a saturated aqueous sodium bicarbonate solution and saline. The organic layer thus obtained was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The concentrated solid was added with a mixed solution of ethyl acetate/hexane (1/1), and stirred for 2 hours or more. The resulting solid was filtered under reduced pressure, washed with diethyl ether, and the filtered solid was dried with warm wind in an oven (40° C.) for 3 hours or more to obtain the title compound (3.9 g, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09388165B2 |
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| Source dataset | uspto-grants-2016_07 |
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| ORD ID | ord-f6c346b5bc3b47c4b48e3f2c31084e5c |
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| Source note | uspto-grants-2016_07 |
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