HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 9880446, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 10292092 | HCID 10292092 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9880446 | HCID 9880446 | 51.9% |
Reaction Steps
A solution of 2.89 g (8.0 mmol) of 5-chloro-2-(3,4-dimethoxybenzyl)-7-(3-hydroxy-propyl)-benzoxazole in 50 ml of THF and 1.23 ml (8.8 mmol) of triethylamine and with 0.58 g of 10% Pd-C was hydrogenated in an autoclave at about 1100 psi. After 2.5 hour, the catalyst was filtered off and the solvents evaporated in vacuo. The residue was dissolved in dichloromethane and filtered through 6.3 g of silica gel in a column. The recovered material (2.53 g) was crystallized from di-isopropyl ether to give the title compound (1.36 g, 51.9%), mp 95-7° C. A second crop of 0.94 g (35.9%) was also obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06372770B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-8be22fd3887245fc9e7797c8ae139fe0 |
| Source note | uspto-grants-2002_04 |