HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron tribromide → (2R,3R,4R,5S,6S)-2-(acetoxymethyl)-6-(4-chloro-3-(4- hydroxybenzyl)phenyl)tetrahydro-2H-pyran-3,4,5-triyl triacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | (2R,3R,4R,5S,6S)-2-(Acetoxymethyl)-6-[4-chloro-3-(4-ethoxybenzyl)phenyl]tetrahydro-2H-pyran-3,4,5-triyl triacetate | HCID 10415783 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (2R,3R,4R,5S,6S)-2-(acetoxymethyl)-6-(4-chloro-3-(4- hydroxybenzyl)phenyl)tetrahydro-2H-pyran-3,4,5-triyl triacetate | HCID 67115824 | 76.2% |
Reaction Conditions
| Temperature | -30 °C |
|---|
Reaction Steps
To a stirred solution of acetic acid (2R,3R,4R,5S,6S)-3,4,5-triacetoxy-6-[4-chloro-3-(4-ethoxy-benzyl)-phenyl]-tetrahydro-pyran-2-ylmethyl ester (4.0 g, 6.93 mmol) prepared using the procedures described in J. Med. Chem. 2008, 51(5), 1145-49, in dichloromethane (40 mL) was added 1 molar solution of BBr3 (34.6 mL, 34.6 mmol) at −78° C. under nitrogen atmosphere. Reaction was stirred at −78° C. for 1.5 h and −30° C. for 1 h. Reaction mixture was poured over ice and neutralized with sat. NaHCO3 (20 mL), extracted with dichloromethane, concentrated and purified by silica gel column chromatography to furnish acetic acid (2R,3R,4R,5S,6S)-3,4,5-triacetoxy-6-[4-chloro-3-(4-hydroxy-benzyl)-phenyl]-tetrahydro-pyran-2-ylmethyl ester (2.9 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08466114B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-de553ed05bbf457d801274a75954c91c |
| Source note | uspto-grants-2013_06 |