HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 9816246, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 9794544 | HCID 9794544 | — |
| Reactant | HCID 178418573 | HCID 178418573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9816246 | HCID 9816246 | 86% |
Reaction Steps
To a solution of N-(1-formyl-1-methylethyl)-2,4-difluorobenzamide obtained in Example 32 (1.14 g, 5 mmol) in THF (10 ml) was added 0.9 M methyl magnesium bromide in THF (13 ml, 12 mmol) dropwise at −20° C. The reaction mixture was warmed gradually to room temperature over 2 hours and added to 10% aqueous ammonium chloride (100 ml). The resulting mixture was extracted with ethyl acetate, washed with saturated aqueous NaHCO3 and brine, dried over MgSO4, concentrated under a reduced pressure and the residue was crystallized from hexane/ethyl acetate to give the title compound (1.05 g; 86%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06936736B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-688bda6e980d489f9768ef365b69f0fd |
| Source note | uspto-grants-2005_08 |