HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 58231453, compound → HCID 58231449, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 58231453 | HCID 58231453 | — |
| Reactant | HCID 178418373 | HCID 178418373 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58231449 | HCID 58231449 | 60% |
Reaction Steps
To the stirred and cold solution (0° C.) of N-methoxy-N-methyl-3-(2,4,6-trichloro-phenyl)-propionamide (1 g, 3.37 mmol) in THF (15 ml) kept under nitrogen atmosphere, MeMgI (1.3 mL of 3M ether solution, 3.9 mmole) was added and stirring was continued at 0° C. for 2 hours. Reaction mixture was quenched with 5% of HCl (10 ml) at 0° C. and aqueous layer was extracted with EtOAc (3×30 ml). The combined organic layer was washed with 20 ml of brine and dried over sodium sulfate; concentrated under vacuum to give off-white solid. The residue was purified by chromatography over silica gel. 0.50 g (60.0% of theory) of 4-(2,4,6-trichloro-phenyl)-butan-2-one was obtained in form of a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08258169B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-be22f3f47f6141f6a926ec263c41b39b |
| Source note | uspto-grants-2012_09 |