Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 54411816 | HCID 54411816 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 53685887 | HCID 53685887 | — |
Reaction Steps
Sodium (356 mg) was dissolved in 20 ml of methanol and 900 mg of N-[6-chloro-5-(4-methoxycarbonyl-2-propylphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide was added thereto with stirring at room temperature. The reaction mixture was stirred at room temperature for five hours and forty minutes, at 60° C. for one hour and fifty minutes and at room temperature overnight. After that, the mixture was poured into a mixture of IN hydrochloric acid and ice. Crystals separated out therefrom were collected by filtration and the resulting crystals were purified by a silica gel column chromatography (chloroform-ethanol=20:1). The resulting amorphous substance was crystallized in ether and collected by filtration to give 452 mg of N-[6-methoxy-5-(4-methoxycarbonyl-2-propylphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06083955 |
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| Source dataset | uspto-grants-2000_07 |
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| ORD ID | ord-51425a934043432a807d5a3fc1d8ec7d |
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| Source note | uspto-grants-2000_07 |
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