Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Dithionite | HCID 24489 | — |
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 19437772 | HCID 19437772 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19437742 | HCID 19437742 | — |
Reaction Steps
A suspension of 1.0 g (2.94 mmol) of 7-benzyloxy-1-isobutyl-2-methyl-3-nitropyrrolo [2,3-d]pyridazine in 30 ml of methanol is treated with a solution of 2.6 g (14.6 mmol) of sodium dithionite in 30 ml of water and stirred at 70° C. for 30 min. After addition of 100 ml of water, the mixture is extracted with 3×100 ml of ethyl acetate. The organic extracts are washed with 200 ml of water, dried over magnesium sulfate and subsequently treated with a solution of 341 mg (2.94 mmol) of fumaric acid in 10 ml of methanol. The solution is subsequently concentrated to a volume of 30 ml. After filtration, 800 mg (64%) of the title compound are isolated. M.p.: 143° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05534515 |
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| Source dataset | uspto-grants-1996_07 |
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| ORD ID | ord-58564a1ea33c4994bc3b0b5acbeab9cc |
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| Source note | uspto-grants-1996_07 |
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