Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 19081411 | HCID 19081411 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 23203297 | HCID 23203297 | — |
Reaction Steps
Into 3 ml of a trifluoroacetic acid solution of 0.22 g of 2-tert-butyl-4-(4-methyl-1,3-dioxan-2-yl)-5-(4-pyridylmethylamino)pyridazin-3-(2H)-one obtained in Preparation Example 4 (2), 0.5 ml of deionized water was thoroughly dropwise added at room temperature. The mixture was stirred at room temperature for one hour. Then, 80 ml of ethyl acetate was added to the system, and the mixture was washed with a saturated sodium chloride aqueous solution. Then, the ethyl acetate layer was dried over anhydrous sodium sulfate, and the solvent was distilled off. The residue was subjected to column chromatography, and using an eluent (ethyl acetate:methanol=40:1), 0.15 g of the desired product (Compound No. 24) having a melting point of from 90° to 93° C. was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05763439 |
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| Source dataset | uspto-grants-1998_06 |
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| ORD ID | ord-926f258efb054d2aa31180d973e030ae |
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| Source note | uspto-grants-1998_06 |
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