HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium methanesulfinate → HCID 57656374, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium methanesulfinate | HCID 2733271 | — |
| Reactant | HCID 57656525 | HCID 57656525 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57656374 | HCID 57656374 | — |
Reaction Steps
To the crude 3-tert-butoxycarbonyl-6-(4-bromomethyl-benzylthio)-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine in anhydrous DMF (1 mL) under nitrogen, add with string sodium methanesulfinate (400 mg, 3.9 mmol), and continue stirring for 30 min at ambient temperature followed by 2 h at 40° C. Add water, extract three times with EtOAc, wash with brine, dry over anhydrous MgSO4, and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (3:1) to give a clear oil that solidifies on standing to a white solid (118 mg, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022062B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-18e5611b45364eeaab35cbd0e20d7272 |
| Source note | uspto-grants-2011_09 |