HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenemethanamine, 3,4-dichloro- → HCID 59392885, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenemethanamine, 3,4-dichloro- | HCID 1608 | — |
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 58100961 | HCID 58100961 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59392885 | HCID 59392885 | 44% |
Reaction Steps
N,N′-Dicyclohexylcarbodiimide (110 mg, 0.522 mmol) was added to a stirred solution of the product from Example 19.6 (200 mg, 0.475 mmol) in dichloromethane (100 mL), After 30 min, N,N-dimethylaminopyridine (6 mg, 0.05 mmol), 3,4-dichlorobenzylamine (92 mg, 0.52 mmol) and 1-hyroxybenzotriazole (70 mg, 0.52 mmol) were added successively. The mixture was stirred at room temperature overnight and aqueous work-up and extraction afforded the crude product was further purified by column chromatography (hexane/ethyl acetate 4:1) as eluent to afford the desired product (120 mg, 44%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08859563B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-9c503500584e4a619662a37f1322ba3d |
| Source note | uspto-grants-2014_10 |