Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Chlorobenzoyl chloride | HCID 8501 | — |
| Reactant | Tin tetrachloride | HCID 24287 | — |
| Reactant | HCID 22632516 | HCID 22632516 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86589889 | HCID 86589889 | — |
Reaction Steps
1.5 g (4.7 mol) of ethyl[((1-benzyl-4-nitro-1H-pyrazol-3-yl)methyl)amino]acetate was dissolved in 50 ml of dichloromethane: 0.71 ml (5.6 mmol) of 4-chlorobenzoyl chloride and 0.85 ml (6.1 mmol) of triethylamine were added to the obtained solution under cooling with ice, and they were stirred under cooling with ice for 2 hours. After the treatment with dichloromethane as the extracting solvent by an ordinary method, the obtained crude product was dissolved in 100 ml of ethanol. 5.3 g (23.5 mmol) of tin chloride was added to the obtained solution, and they were stirred at 70° C. overnight. The solvent was evaporated. Sodium carbonate and ethyl acetate were added to the residue, and they were vigorously stirred at room temperature. After the treatment with ethyl acetate as the extracting solvent by an ordinary method, the obtained crude product was purified by the silica gel column chromatography to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06825191B2 |
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| Source dataset | uspto-grants-2004_11 |
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| ORD ID | ord-4b43f89a434744f1b715502af795cf2d |
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| Source note | uspto-grants-2004_11 |
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