Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 58531010 | HCID 58531010 | — |
| Product | HCID 76814748 | HCID 76814748 | — |
Reaction Steps
There was suspended, in ethanol (2 mL), 5-chloro-2-(4-chloro-phenyl)-7-morpholin-4-yl-pyrazolo[1,5-a]pyrimidine (50.0 mg, 0.143 mM) and then potassium carbonate (21.7 mg, 0.157 mM) and hydrazine monohydrate (69.4 μL, 1.43 mM) were added to the suspension. This suspension was stirred at 150° C. for 20 minutes, while applying microwaves to the same. This reaction liquid was diluted with a saturated aqueous common salt solution and then extracted with ethyl acetate. The extracts thus obtained were combined together and then dried over anhydrous sodium sulfate and the solvent was distilled off. The resulting residue was suspended in ethanol (2 mL), then acetic acid (5.0 μL, 0.087 mM) and 3-methyl-benzaldehyde (17.0 μL, 0.144 mM) were added to the suspension and the mixture was stirred at room temperature for one hour. This reaction liquid was filtered and the resulting solid was purified by the NH-silica gel column chromatography (methylene chloride) to give the title compound (36.8 mg, overall yield of these two steps: 58%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08314098B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-99ff8ac9c970440888a4daa74936f5f0 |
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| Source note | uspto-grants-2012_11 |
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