HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 68752580, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ozone | HCID 24823 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 67026987 | HCID 67026987 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68752580 | HCID 68752580 | — |
Reaction Steps
To a solution of tert-butyl 5,6-diethenylpyridine-3-carboxylate (19.0 g, 82 mmol) in dichloromethane (821 mL) at −78° C. was added ozone gas. The ozone bubbled though the solution until saturated (1 h). Nitrogen gas was then bubbled through the solution. The mixture was diluted with methanol (821 mL) and sodium borohydride (7.77 g, 205 mmol) was added. After 15 min, the mixture was quenched with saturated aqeuous sodium bicarbonate and washed with dichloromethane (3×). The combined organics were washed with brine, dried with magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% dichloromethane→15% methanol/dichloromethane) gave the title compound. MS: m/z=240.3 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08754096B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-89f66082272f45f3b145351584fa1cd2 |
| Source note | uspto-grants-2014_06 |