Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | Methanesulfonamide | HCID 72879 | — |
| Reactant | 1,4-Bis(dihydroquinidine)phthalazine | HCID 11217202 | — |
| Reactant | HCID 67276589 | HCID 67276589 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 68710189 | HCID 68710189 | 89% |
Reaction Steps
Ad-mix-β (28.0 g) and methanesulfonamide (1.90 g, 20 mmol) were suspended in t-butanol (100 mL) and water (100 mL), then the compound (7.7 g, 20 mmol) synthesized in the above (2) was added under stirring with cooling with ice. The reaction solution was stirred for 15 hours with cooling with ice, then sodium sulfite (20 g, 0.16 mol) was added, and further stirred at room temperature for 1 hour. The reaction solution was poured in water, extracted with chloroform, and the organic layer was washed with saturated ammonium chloride and dried with magnesium sulfate. The solvent was removed under reduced pressure, and the resulting pale yellow solid was washed with diisopropyl ether and n-heptane to obtain the entitled compound (5.1 g, 89%) as a milky white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08163770B2 |
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| Source dataset | uspto-grants-2012_04 |
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| ORD ID | ord-40ca6fd5f49a475bb53cffa48b752b41 |
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| Source note | uspto-grants-2012_04 |
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