HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclopropylamine → N-(4-Chloro-3-cyclopropylaminomethyl-benzyl)-3,3,3-trifluoro-propionamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclopropylamine | HCID 69828 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | N-(4-Chloro-3-formyl-benzyl)-3,3,3-trifluoro-propionamide | HCID 86622955 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | N-(4-Chloro-3-cyclopropylaminomethyl-benzyl)-3,3,3-trifluoro-propionamide | HCID 67148430 | 96.5% |
Reaction Steps
A mixture of N-(4-chloro-3-formyl-benzyl)-3,3,3-trifluoro-propionamide (840 mg, 3.00 mmol) and cyclopropylamine (0.320 mL, 4.51 mmol) in MeOH (30 mL) was heated to reflux for 4 h. The mixture was allowed to cool to rt. NaBH4 (170 mg, 4.51 mmol) was added in portions. The mixture was stirred for 1 h, and the solvents were removed under reduced pressure. The residue was diluted with EtOAc, and the resulting mixture was washed with aq. sat. NaHCO3 and brine. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (CH2Cl2/MeOH 90:10) yielded the title compound (929 mg, 96%). LC-MS: tR=0.64 min; ES+: 321.05.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07799805B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-71cd3e9d34ce4a63be11a1abb898a174 |
| Source note | uspto-grants-2010_09 |