Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22989423 | HCID 22989423 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 22989358 | HCID 22989358 | 34.1% |
Reaction Steps
458 mg of ethyl 2-[3-chloro-6-[3-[4-(diphenylmethyl)piperazino]propoxy]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate trihydrochloride was dissolved in 4 ml of 2-propanol; 1.34 ml of a 2 N aqueous solution of sodium hydroxide was added, followed by stirring at 80° C. for 1.5 hours, after which 0.3 ml of a 2 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 2 hours. After cooling, the mixture was concentrated under reduced pressure; the residue was diluted with water and washed with ethyl acetate; the water layer was ajusted to pH 4 by the addition of 1 N hydrochloric acid, followed by extraction with ethyl acetate; the extract was dried with sodium sulfate. The dry product was concentrated under reduced pressure and crystallized by the addition of ethyl acetate-ethyl ether-hexane (2:5:1), collected by filtration, washed with ethyl ether and dried to yield 125 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06248740B1 |
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| Source dataset | uspto-grants-2001_06 |
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| ORD ID | ord-46c5180577f24daab0ae435ebf35c9e0 |
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| Source note | uspto-grants-2001_06 |
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