HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → N-[4-methoxybenzenesulfonyl]-(D)-asparagine methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | N-[4-methoxybenzenesulfonyl]-(D)-asparagine | HCID 27014145 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | N-[4-methoxybenzenesulfonyl]-(D)-asparagine methyl ester | HCID 70060643 | — |
Reaction Steps
N-[4-methoxybenzenesulfonyl]-(D)-asparagine (10.1 g, 33.3 mmol) is dissolved in dimethylformamide (167.0 mL). Cesium carbonate (5.43 g, 16.66 mmol) is added, followed by the addition of methyl iodide (2.22 mL, 33.3 mmol), and the reaction is stirred overnight. The reaction is then diluted with saturated ammonium chloride (366.0 mL), and extracted well with ethyl acetate. The combined organic extracts are washed with brine, dried (Na2SO4), and the solvent is evaporated. The crude product is recrystallized from toluene to provide N-[4-methoxybenzenesulfonyl]-(D)-asparagine methyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05552419 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-bcee4949359347dba38b761ba6fdba32 |
| Source note | uspto-grants-1996_09 |