HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 67073443, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 67073052 | HCID 67073052 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67073443 | HCID 67073443 | — |
Reaction Steps
To a solution of 7.5 g of ((S)-2-[(4-benzyloxy-2,5-difluoro-phenyl)-hydroxy-methyl]-morpholine-4-carboxylic acid tert-butyl ester in dichloromethane (90 ml) was added with cooling (0-5° C.) tetrabromomethane (12.5 g) and afterwards triphenylphosphine (13.5 g) in small portions. Stirring continued for 1 hour at room temperature before the mixture was added dropwise to diethyl ether (600 mL). Solids were removed by filtration and the filtrate was concentrated in vacuo. The residue was then purified by column chromatography (heptane-ethyl acetate (3:1)/silica gel) to give 5.6 g of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07323466B2 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-e551579a49474d7198c5c2a3fe32e69b |
| Source note | uspto-grants-2008_01 |