Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclopropylamine | HCID 69828 | — |
| Reactant | HCID 18466614 | HCID 18466614 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18466610 | HCID 18466610 | 75% |
Reaction Steps
A solution of 5-bromo-2-chloro-N-(2,6-dichloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide (3.00 g, 7.61 mmol) and cyclopropylamine (2.11 mL, 30.5 mmol) in xylenes was heated in a sealed tube at 120° C. for 24 h. The reaction was cooled to 0° C., diluted with water and extracted with EtOAc (2×). The combined organic extracts were dried (MgSO4), filtered and concentrated under reduced pressure. The resulting residue was purified by trituration (Et2O:hexane, 3:1) to give the title compound (2.35 g, 75% yield) as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06420359B1 |
|---|
| Source dataset | uspto-grants-2002_07 |
|---|
| ORD ID | ord-3d8dbda2bf32418b8fafdd878830094b |
|---|
| Source note | uspto-grants-2002_07 |
|---|