HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → alpha-[2-(Dimethoxymethyl)phenyl]-3-pyridinemethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | 3-Pyridinecarboxaldehyde | HCID 10371 | — |
| Reactant | 1-Bromo-2-(dimethoxymethyl)benzene | HCID 11148943 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | alpha-[2-(Dimethoxymethyl)phenyl]-3-pyridinemethanol | HCID 14820335 | 99.9% |
Reaction Steps
To a stirred and cooled (-78° C.) mixture of 50 parts of 1-bromo-2-(dimethoxymethyl)benzene and 245 parts of 1,1'-oxybisethane were added dropwise 59 parts of a 1-butyllithium solution 2.5M in hexane. Upon complete addition, stirring was continued for 10 minutes at room temperature. A solution of 23.1 parts of 3-pyridinecarboxaldehyde in 42 parts of 1,1'-oxybisethane was added dropwise to the reaction mixture. Upon completion, the mixture was allowed to reach room temperature. The mixture was taken up in ice water and the product was extracted with 1,1'-oxybisethane. The extract was dried, filtered and evaporated, yielding 56 parts (99.9%) of α-[2-(dimethoxymethyl)phenyl]-3-pyridinemethanol as a residue (intermediate 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04746671 |
| Source dataset | uspto-grants-1988_05 |
| ORD ID | ord-2635f8c911bf4625b97ce2649a33c245 |
| Source note | uspto-grants-1988_05 |