HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosgene → 4-[(1S,7S,7aR)-7-tert-Butyldimethylsilanoxy-1-methyl-3-oxo-hexahydro-pyrrolo[1,2-c]imidazol-2-yl]-2-chloro-3-methylbenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 66863531 | HCID 66863531 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-[(1S,7S,7aR)-7-tert-Butyldimethylsilanoxy-1-methyl-3-oxo-hexahydro-pyrrolo[1,2-c]imidazol-2-yl]-2-chloro-3-methylbenzonitrile | HCID 16733764 | — |
Reaction Steps
To a solution of crude 61I (˜1.81 mmol) in CH2Cl2 (10 mL) was added i-Pr2NEt (2 mL) followed by 20% phosgene in toluene (2.5 mL) dropwise. The reaction was stirred at rt overnight. Reaction was extracted with EtOAc (50 mL) which was washed twice with 1N HCl and then saturated NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated. Purification by flash chromatography (silica gel, 0 to 10% EtOAc in hexane) provided the title compound (369 mg): MS (ES) m/z 420.23 [M+H]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07772267B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-b5cad3ea43654e2ab14008575578c41a |
| Source note | uspto-grants-2010_08 |