HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 10703983, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 3-(Methylamino)propanoic acid, N-BOC protected | HCID 2760952 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10703983 | HCID 10703983 | 99.2% |
Reaction Steps
To a solution of 3-(tert-butoxycarbonyl(methyl)amino)propanoic acid (7.0 g, 0.032 mol) and K2CO3 (13.3 g, 0.096 mol) in DMF (100 mL) was added MeI (9.0 g, 0.064 mol) at rt. The resultant solution was stirred at rt for 3 hrs. The reaction mixture was quenched with ice water and extracted with ethyl acetate (2×). The combined organic layer was dried over Na2SO4, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (gradient elution 0%˜10% EtOAc/petroleum ether) to afford methyl 3-(tert-butoxycarbonyl (methyl) amino)propanoate (6.9 g, 92%) as a white solid. ESI-MS (EI+, m/z): 118 [M-100+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08962843B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-05638209dcf14683a4a20efa2d82cd4e |
| Source note | uspto-grants-2015_02 |