HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 59840082, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 59840130 | HCID 59840130 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59840082 | HCID 59840082 | 46.4% |
Reaction Steps
To a stirred solution of carbonic acid ditrichloromethyl ester (triphosgene) (31 mg, 0.10 mmol) in CH2Cl2 (5 ml) at 0° C., was added a solution of rac-2-(3,5-bis-trifluoromethyl-phenyl)-N-[(3S,4R)-4-(4-fluoro-phenyl)-pyrrolidin-3-yl]-N-methyl-isobutyramide (Intermediate VII-4), (100 mg, 0.21 mmol) and pyridine (0.02 ml, 0.22 mmol) in CH2Cl2 (2 ml) over 30 minutes. The temperature was raised to RT, and stirring was continued for 2 hours. The organic phase was washed with H2O, dried over Na2SO4. Purification by flash chromatography (SiO2, EtOAc/Hx 1:1) yielded 25 mg (22%) of the title compound as_colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07893062B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-6d0fb5d11ff148b7aa1cb6afc64303f9 |
| Source note | uspto-grants-2011_02 |