HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → (2S,4R)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-4-(3-fluoro-5-nitrophenoxy)pyrrolidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1,3-Difluoro-5-nitrobenzene | HCID 75272 | — |
| Reactant | HCID 11174939 | HCID 11174939 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | (2S,4R)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-4-(3-fluoro-5-nitrophenoxy)pyrrolidine-1-carboxylate | HCID 59751405 | 66% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a 0° C. solution of (2S,4R)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-4-hydroxypyrrolidine-1-carboxylate (1 equiv) in DMF (0.5 M) was added NaH (1.3 equiv) as a solid. After stirring for 30 minutes at 0° C., 3,5-difluoronitrobenzene (1.2 equiv) was added by syringe. The reaction mixture was allowed to warm to room temperature and stirred overnight. The reaction was quenched by the addition of water, and the mixture was diluted with EtOAc. The organic layer was washed four times with water and once with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. Purification by flash chromatography (10-20% EtOAc/Hexanes) provided the title compound in 66% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07538223B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-bcf06f7e1f8841cb9057c9ca80a55358 |
| Source note | uspto-grants-2009_05 |