HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 14989563, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | 5-Bromo-2-hydroxypyridine | HCID 599528 | — |
| Reactant | Triisopropylsilyl trifluoromethanesulfonate | HCID 2724529 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14989563 | HCID 14989563 | 100.7% |
Reaction Steps
Triisopropylsilyl trifluoromethanesulfonate (65.4 g) was added dropwise to a solution of 5-bromo-2(1H)-pyridinone (33.8 g) and 2,6-lutidine (31.1 g) in 775 ml of dichloromethane at 0° C. The resulting solution was stirred for 15 minutes, and then it was poured into water and the layers were separated. The aqueous phase was extracted with dichloromethane, and the combined organic layers were dried over magnesium sulfate and concentrated to give a liquid. The product was slurried with silica gel and hexanes. Filtration gave 64.6 g of oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05039809 |
| Source dataset | uspto-grants-1991_08 |
| ORD ID | ord-9b43eddfbf6d4f21920eaaf0a3fdbcb2 |
| Source note | uspto-grants-1991_08 |