Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 135554909 | HCID 135554909 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22902388 | HCID 22902388 | — |
Reaction Steps
100 mg of 3-{2-[N-(2-(4-chlorophenyl)-ethyl)-N-methylamino]-ethyloxy}-5-(4-hydroxyphenyl)-2-methylpyrazole (preparation see Example 9) were dissolved in 2 ml of dichloromethane. 0.15 ml of pyridine and 1 ml of acetic anhydride were added to the solution and the reaction mixture was stirred at room temperature for 24 hours. The reaction mixture was subsequently evaporated under reduced pressure, and the residue was taken up in aqueous sodium bicarbonate solution and extracted with dichloromethane. The organic phase was separated, dried and concentrated. The crude title compound which remained as a residue was taken up in tert-butyl methyl ether. To form a salt, a 2N solution of hydrochloric acid in isopropanol was added. The precipitated salt was separated. 80 mg of the hydrochloride of the title compound were obtained having a melting point of from 160° to 175° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05679699 |
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| Source dataset | uspto-grants-1997_10 |
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| ORD ID | ord-b6a0a0fc25784916a73d9571dce47203 |
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| Source note | uspto-grants-1997_10 |
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