Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 10428804 | HCID 10428804 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10763816 | HCID 10763816 | 82.5% |
Reaction Steps
To a solution of N-(1-benzyl-4-methylhexahydro-1H-1,4-diazepin-6-yl)-1H-indazole-3-carboxamide (1.0 g) in dichloromethane (10 ml), acetic anhydride (0.56 g) is added; and the mixture is stirred at 25° C. for 16 hours. The reaction mixture is washed with saturated sodium bicarbonate and dried over sodium sulfate. The solvent is evaporated under reduced pressure, and the residue is chromatographed on silica gel with elution of acetone. Fractions containing the title compound are pooled and evaporated under reduced pressure to give the title compound (0.92 g) as an oil. The free base thus obtained is converted to the fumarate 1/4 hydrate of the title compound in a usual manner, m.p. 166-168° C. (recrystallized from ethanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05017573 |
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| Source dataset | uspto-grants-1991_05 |
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| ORD ID | ord-55381c5c23cc40f399c5e8db041a9230 |
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| Source note | uspto-grants-1991_05 |
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