HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoic Acid → (2S,3R)-N-tert-Butoxycarbonyl-3-benzoyloxy-2-pyrrolidinecarboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoic Acid | HCID 243 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Reactant | 1-tert-butyl 2-methyl (2S,3S)-3-hydroxypyrrolidine-1,2-dicarboxylate | HCID 14729253 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (2S,3R)-N-tert-Butoxycarbonyl-3-benzoyloxy-2-pyrrolidinecarboxylic acid methyl ester | HCID 58583618 | 94.2% |
Reaction Steps
To a solution of 7A (13.5 g, 55 mmol) in anhydrous THF (500 mL) was added triphenylphosphine (26 g, 99 mmol), followed by benzoic acid (10.1 g, 82.7 mmol) and DEAD (9.5 mL, 60 mmol). The reaction mixture was stirred at RT for 2 hours, then partitioned between water and CH2Cl2. The organic phase was washed with saturated aqueous NaHCO3 and brine, dried over Na2SO4 and filtered. The filtrate was concentrated under reduced pressure to give a crude product, which was chromatographed (silica gel) eluting with 15% EtOAc/hexane to give 18.1 g of the title compound as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06670386B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-d12d536c3fcc499783346596473c3aa3 |
| Source note | uspto-grants-2003_12 |