HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 137330059, compound → HCID 137330058, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 137330059 | HCID 137330059 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 137330058 | HCID 137330058 | — |
Reaction Steps
To a solution of (2S,5R)-1-benzyl-5-(tert-butyl-dimethyl-silanyloxymethyl)-pyrrolidine-2-carboxylic acid (3-trifluoromethoxy-phenyl)-amide (97 mg, 0.19 mmol) in THF (1 mL) was added Pd/C (10%, 20 mg). The solution was degassed 3 times replacing air by nitrogen and finally nitrogen by hydrogen. The reaction mixture was further stirred under hydrogen atmosphere overnight. The catalyst was removed through a pad of Celite and washed with THF. Solvent was concentrated and the crude residue was purified by preparative HPLC (Waters SunFire C18-ODB 5 μm, 19×50, 5-100% CH3CN/H2O in 17 min, 100% CH3CN for 3 min, CH3CN and H2O containing 0.1% TFA, flow: 20 mL/min) to give the desired compound. MS (LC/MS): 419 [M+H]+; tR (HPLC conditions b): 5.28 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085555B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-eabb8627949a458ea9a69acc8b8d46ff |
| Source note | uspto-grants-2015_07 |