HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 53255905, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| Reactant | tert-Butyl (3S)-3-hydroxypyrrolidine-1-carboxylate | HCID 854055 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 53255905 | HCID 53255905 | 98% |
Reaction Steps
A solution of (S)-3-hydroxy-pyrrolidine-1-carboxylic acid tert-butyl ester (500 mg, 2.67 mmol) in anhydrous tetrahydrofuran (10 mL) was added to sodium hydride (60% in mineral oil, 215 mg, 5.34 mmol) gradually, and the resulting mixture was stirred at room temperature for 1 h. 2-Chloro-5-nitropyridine (425 mg, 2.68 mmol) was added, and the reaction mixture was stirred at room temperature for 3 h, then quenched with water, extracted with ethyl acetate, washed with water, dried over anhydrous sodium sulfate, and concentrated to afford (S)-3-(5-nitro-pyridin-2-yloxy)-pyrrolidine-1-carboxylic acid tert-butyl ester as a brown oil (800 mg, 98% yield). The NMR spectrum obtained on the sample is compatible with its structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08058299B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-44ae5070f31d4a79b67593f41fed63bc |
| Source note | uspto-grants-2011_11 |