HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 68495138, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 11289510 | HCID 11289510 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 68495138 | HCID 68495138 | 93.3% |
Reaction Steps
To a solution of 4-[(2,2-dimethylpropyl)(2-oxoethyl)amino]-2-(trifluoromethyl)benzonitrile (0.882 g, 2.96 mmol) in MeOH (10 mL) at 0° C. was added NaBH4 (0.112 g, 2.96 mmol) in one portion and the mixture was stirred overnight, slowly warming to rt. The mixture was cooled to 0° C., sat'd NH4Cl (1 mL) was added and the mixture was concentrated in vacuo. The residue was partitioned between EtOAc/water and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (EtOAc/hexanes), affording 0.829 g of the title compound as a colorless syrup which solidified on standing: MS (ESI) m/z 301 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834063B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-1f11d0d3edd148cf8f97c2f27e396e6d |
| Source note | uspto-grants-2010_11 |