HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22882495, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Triisopropylsilyl trifluoromethanesulfonate | HCID 2724529 | — |
| Reactant | HCID 14680532 | HCID 14680532 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22882495 | HCID 22882495 | — |
Reaction Steps
15.4 ml of triisopropylsilyl triflate are added to a solution of 8.7 g of (R)-4-bromo-3-methylbutan-1-ol in 320 ml of methylene chloride at 0° C., and 6.6 ml of 2,6-lutidine are then added in the course of 30 min. The reaction mixture is subsequently poured onto 100 ml of ice-water and the aqueous phase is acidified by addition of 2N hydrochloric acid (pH 3). It is extracted with methylene chloride and the organic phase is washed with a 5% sodium bicarbonate solution and saturated sodium chloride solution and dried over sodium sulfate. After purification of the crude product by FC over 200 g of silica gel (mobile phase J), the title compound is obtained: Rf (J)=0.48.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05719141 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-721540f4c86945ceb4ddaff8aeba780f |
| Source note | uspto-grants-1998_02 |