HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron trifluoride etherate → HCID 18662976, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron trifluoride etherate | HCID 8000 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | HCID 23226991 | HCID 23226991 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 18662976 | HCID 18662976 | 31.5% |
Reaction Steps
A solution of 500 mg of 5-(2,2-dimethyl-7-fluoroindan-3-on-1-yl)-4-methylthiopyrimidine, 5.0 g of triethylsilane and 3.0 g of boron trifluoride etherate in 20 mL of 1,2-dichloroethane was heated to reflux with stirring for 16 hr. The resulting solution was cooled and then poured into an aqueous solution of sodium carbonate. The mixture obtained was extracted with ether and the ethereal extract was dried over magnesium sulfate, filtered, and concentrated by evaporation under reduced pressure. The residue was purified by column chromatography on silica gel to obtain a colorless oil. A portion of this oil was crystallized from hexane to obtain 150 mg of the title compound as a white solid melting at 81°-82° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05780465 |
| Source dataset | uspto-grants-1998_07 |
| ORD ID | ord-89854b0613a24981ac53c521853d7a3e |
| Source note | uspto-grants-1998_07 |