HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 3-(s)-[(Benzyloxycarbonyl)amino]-2-(r,s)-acetoxy-4-methyl pentanoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 131720810 | HCID 131720810 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-(s)-[(Benzyloxycarbonyl)amino]-2-(r,s)-acetoxy-4-methyl pentanoic acid | HCID 131720811 | 80% |
Reaction Steps
To a solution of 3-(S)-[(benzyloxycarbonyl)amino]-2-(R,S)-hydroxy-4-methylpentanoic acid (1.70 g, 6.04 mmol) and pyridine (4.9 mL) was added acetic anhydride (5.7 mL, 6.17 g, 60.4 mmol) dropwise at room temperature. The reaction was allowed to stir overnight and was diluted with ethyl acetate and washed with water (2×). The organic layer was dried over magnesium sulfate, filtered and evaporated in vacuo to give a thick oil. The residue was purified by column chromatography on silica gel with 15% methanol/dichloromethane to afford 1.56 g (80%) of 3-(S)-[(benzyloxycarbonyl)amino]-2-(R,S)-acetoxy-4-methyl pentanoic acid as a light yellow viscous oil. FAB MS [M+H] m/z; Calcd: 324, Found: 324.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06656910B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-9532da9613a44d029086081c5dcf1349 |
| Source note | uspto-grants-2003_12 |