HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenemethanamine, 3-chloro- → HCID 54004440, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenemethanamine, 3-chloro- | HCID 77802 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Reactant | HCID 10355503 | HCID 10355503 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 54004440 | HCID 54004440 | — |
Reaction Steps
To a solution of 3-chlorobenzylamine (0.628 mL, 5.14 mmol) and crushed molecular sieves (1.5 g) in dichloroethane (10 mL) under nitrogen at 0° C. was added sodium triacetoxyborohydride (2.73 g, 12.9 mmol), followed the product from Step C (2.73 g, 5.14 mmol). The reaction was stirred overnight, allowing it to warm to room temperature. The solution was poured into EtOAc and sat NaHCO3 solution, and the organic layer was washed with brine, dried (Na2SO4), filtered, and concentrated in vacuo to provide the crude product which was purified by silica gel chromatography (2.5-5% MeOH/CHCl3) to obtain the titled compound as a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05756528 |
| Source dataset | uspto-grants-1998_05 |
| ORD ID | ord-d0e7c54d4cc440e0ab0a56e62e9e2f5b |
| Source note | uspto-grants-1998_05 |