Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 66603131 | HCID 66603131 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 135845057 | HCID 135845057 | 42% |
Reaction Steps
To 2 ml of dichloromethane solution containing 99 mg (0.21 mmol) of 2-(4-difluoromethoxy-3-isopropoxyphenyl)-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]-pyridazin-4-one obtained in Example 39-(a) was added 0.1 ml of boron trifluoride diethyl ether complex under ice-cooling, and the mixture was reacted at room temperature for 3 hours. After completion of the reaction, methanol and 28% aqueous ammonia were added to the solid obtained by filtrating the reaction suspension, and the mixture was stirred at room temperature for 12 hours. Then, the solution was concentrated under reduced pressure, and the obtained solid was washed with chloroform and dried under reduced pressure to obtain 29 mg of the title compound as a white solid. (Yield: 42%)
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-131c7765f5f04302b89c822c80284073 |
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| Source note | uspto-grants-2013_05 |
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