HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → HCID 15280226, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 15280224 | HCID 15280224 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 15280226 | HCID 15280226 | 84.3% |
Reaction Steps
Add sodium borohydride (0.96 g, 25.4 mmole) to 8-chloro[1]benzoxepino[4,3-b]pyridin-11-one (10.00 g, 40.7 mmole) in ethanol (100 mL). Stir for 18 hours at room temperature. Add water (100 mL), and concentrate in vacuo. Add additional water (100 mL), and extract with dichloromethane. Wash the organic solution with saturated NaCl, dry with MgSO4, filter, and concentrate in vacuo. Dissolve the oil in dichloromethane, and chromatograph on silica gel, eluting with 50% ethyl acetate in hexane. Combine the appropriate fractions, and concentrate under reduced pressure to give a white solid (8.50 g, 84% yield): mp 105°-108° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05430032 |
| Source dataset | uspto-grants-1995_07 |
| ORD ID | ord-e93fbc7317bf44db960518e6992a5706 |
| Source note | uspto-grants-1995_07 |