HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric acid magnesium salt (1:1) → HCID 59204396, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Reactant | HCID 178513265 | HCID 178513265 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ammonia | HCID 222 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59204396 | HCID 59204396 | — |
Reaction Steps
100 mg of 4-{1-(4-fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-2-yl}-N-hydroxybenzamidine (3) were dissolved in 100 ml of tetrahydrofuran and, with 2 ml of conc. ammonia, hydrogenated over Raney nickel at a hydrogen pressure of 75 bar and 25° C. for 30 hours. After addition of magnesium sulfate, the reaction solution was filtered. The filtrate was concentrated and separated by HPLC (Knauer Eurospher-100-10-C18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoro-acetic acid)=80/20→10/90). This gave the product of molecular weight 435.48 (C25H23F2N3O2); MS (ESI): 436.18 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07671047B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-a68b0eaf62e34802b89f76cfd94ff9e4 |
| Source note | uspto-grants-2010_03 |