HuagongsheHuagongshe Chemistry Print Report · For research reference only
(2S,4S)-1-tert-Butyl 2-methyl 4-(((benzyloxy)carbonyl)amino)pyrrolidine-1,2-dicarboxylate → (2S,4S)-4-Benzyloxycarbonylaminopyrrolidine-2-carboxylic Acid Methyl Ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (2S,4S)-1-tert-Butyl 2-methyl 4-(((benzyloxy)carbonyl)amino)pyrrolidine-1,2-dicarboxylate | HCID 57648857 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | (2S,4S)-4-Benzyloxycarbonylaminopyrrolidine-2-carboxylic Acid Methyl Ester | HCID 45072528 | 67.9% |
Reaction Steps
(2S,4S)-4-Benzyloxycarbonylaminopyrrolidine-1,2-dicarboxylic acid 1-t-butyl ester 2-methyl ester (10.4 g, 28 mmol) was dissolved in a 4M solution of HCl in 1,4-dioxane. The solution was stirred at room temperature for 3 hours and then evaporated. The residue was partitioned between EtOAc (200 mL) and 1M NaOH (100 mL), the layers separated and the aqueous layer re-extracted with EtOAc (100 mL). The combined organics were washed with saturated aqueous NaCl (100 mL), dried over Na2SO4, and evaporated to afford the title compound (5.4 g, 19 mmol) as a white solid, which was used without further purification. MS m/z: [M+H]+ calcd for C14H18N2O4, 278.3. found 279.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08106082B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-bd5e82e96cb340c6a5e1d7f5caac4b19 |
| Source note | uspto-grants-2012_01 |