HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 23499504, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 23499489 | HCID 23499489 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23499504 | HCID 23499504 | — |
Reaction Steps
To a solution of 3-(2-benzylsulfonylhydrazino)-1-[(2-ethoxycarbonyl)ethyl]-6-methylpyrazinone, the product of Example 30 (0.398 g, 1.01 mmol), in tetrahydrofuran (10 mL) containing 5% methanol, is added sodium borohydride (0.229 g, 6.07 mmol) at room temperature. The reaction mixture is stirred for 5 hours. Water (2 mL) is then added and the mixture is fractionated between dichloromethane and water. The organic phase is dried over anhydrous sodium sulfate and is concentrated under reduced pressure. The crude residue is purified using silica gel column chromatography with ethyl acetate/n-hexane as eluent to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06777431B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-c46479f8c8844a27a2770c714711f97c |
| Source note | uspto-grants-2004_08 |