HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → 1-(3-Fluoropyridin-2-yl)-3-hydroxycyclobutane-1-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 1-(3-Fluoropyridin-2-yl)-3-oxocyclobutane-1-carbonitrile | HCID 67453141 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(3-Fluoropyridin-2-yl)-3-hydroxycyclobutane-1-carbonitrile | HCID 67453032 | 79.2% |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
To a solution of 1-(3-fluoropyridin-2-yl)-3-oxocyclobutanecarbonitrile (231 g, 1.22 mol) in a mixture of DCM (2 L) and MeOH (200 mL) was added NaBH4 portionwise at −78° C. The reaction mixture was stirred at −78° C. for 1 h and quenched with a mixture of methanol and water (1/1). The organic layer was washed with water (500 mL×3), dried over Na2SO4, and concentrated. The residue was purified on silica gel (50% EtOAc/hexanes) to provide the title compound as an amber oil (185.8 g, 77.5%). LRMS (M+H+) m/z 193.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08962632B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-63e12865e459440f9afdc7323707fdff |
| Source note | uspto-grants-2015_02 |