Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 66602481 | HCID 66602481 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 135620468 | HCID 135620468 | 62% |
Reaction Steps
To 1 ml of dichloromethane solution containing 186 mg (0.367 mmol) of 3-bromo-2-(3-cyclopropoxy-4-methoxyphenyl)-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]-pyridazin-4-one obtained in Example 43-(a) was added 6 ml of 1,4-dioxane solution containing 4N hydrogen chloride, and the mixture was stirred at room temperature for 8 hours. After completion of the reaction, the solid obtained from the reaction suspension by filtration was washed with diisopropyl ether. To the obtained crude solid were added methanol and 28% aqueous ammonia, and the mixture was stirred at room temperature for 5 hours. Then, the solution was concentrated under reduced pressure and the obtained solid was washed with ethyl acetate and dried under reduced pressure to obtain 85 mg of the title compound as a white solid. (Yield: 62%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08450319B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-e3eff324dda44e85bee6865e4fc932b5 |
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| Source note | uspto-grants-2013_05 |
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