HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → HCID 23499507, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 23499504 | HCID 23499504 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23499507 | HCID 23499507 | — |
Reaction Steps
To a magnetically stirred solution of 3-(2-benzylsulfonylhydrazino)-1-(3-hydroxypropyl)-6-methylpyrazinone, the product of Example 31 (0.429 g, 0.82 mmol) and carbon tetrabromide (0.328 g, 0.99 mmol) in dichloromethane (10 mL), is added triphenylphosphine (0.26 g, 0.99 mmol) portionwise with ice-bath cooling. After the addition is complete, the mixture is stirred for about an additional 2 hours. The solvent is removed in vacuo. The residue is purified by silica gel column chromatography using 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-b9e0912b8d8844948d27b8e2d0d41d2b |
| Source note | uspto-grants-2004_08 |