HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 19029808, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Boron Trichloride | HCID 25135 | — |
| Reactant | HCID 19029752 | HCID 19029752 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19029808 | HCID 19029808 | 80% |
Reaction Steps
4 g (8 mmol) of benzyl 2-hydroxy-4-(3-methoxy-5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthoylmethoxy)benzoate and 20 ml of dichloromethane are introduced into a flask. 24 ml (24 mmol) of a solution of boron trichloride in THF (1M) are added dropwise at -78° C. and under a stream of nitrogen and the temperature is allowed to rise to -20° C., then the reaction mixture is poured into ice-water. The mixture is extracted with ethyl ether, and the organic phase is separated, dried over magnesium sulphate and evaporated. The residue obtained in purified by chromatography on a silica column, eluted with a dichloromethane/hexane mixture (50:50). 3.1 g (80%) of the expected ester of melting point 127°-128° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05654331 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-5f223468f0274b0a8d7603fe3de513c3 |
| Source note | uspto-grants-1997_08 |