HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 22254170, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 131725264 | HCID 131725264 | — |
| Reactant | HCID 178418255 | HCID 178418255 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22254170 | HCID 22254170 | 75% |
Reaction Steps
Phenylmagnesiumbromide (1M in THF) (2eq) is added to a solution of 8 (50 mg) in THF (10 ml) at 78° C. under argon with stirring. The reaction is allowed to stir for 15 min. at 78° C. after the addition of Grignard at which time sat; aq. NH4Cl (4 ml) is added to quench the reaction. The mixture is diluted with EtOAc (60 ml) and water (2 ml), and the layers are separated. The organic layer is washed with sat. aq. NH4Cl (10 ml), water (10 ml), brine (10 ml), dried (Na2SO4), filtered and concentrated. The residue is purified by silica column chromatography eluting with EtOAc/hexane to give 13.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06989382B2 |
| Source dataset | uspto-grants-2006_01 |
| ORD ID | ord-dce057c42b7e426a84f1ad480725696e |
| Source note | uspto-grants-2006_01 |