HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → tert-butyl N-{2-[2-(methanesulfonyloxy)ethoxy]ethyl}carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 2-(2-Boc-aminoethoxy)ethanol | HCID 5220470 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | tert-butyl N-{2-[2-(methanesulfonyloxy)ethoxy]ethyl}carbamate | HCID 12106196 | 97.4% |
Reaction Steps
A rapidly stirred solution of tert-butyl 2-(2-hydroxyethoxy)ethylcarbamate (47.1 g, 0.230 mol) in 1 L of anhydrous CH2Cl2 was cooled to 0° C. under N2 and treated with triethylamine (48.0 mL, 0.345 mol). Methanesulfonyl chloride (19.6 mL, 0.253 mol) was then added dropwise over 30 min. The reaction mixture was then allowed to warm to room temperature and was stirred an additional 22 h. The reaction was quenched by addition of 500 mL saturated NaHCO3 solution and the organic layer was separated. The organic phase was then washed with H2O (3×500 mL) and brine. The organic portion was dried over Na2SO4 and concentrated to give 2-{2-[(tert-butoxycarbonyl)amino]ethoxy}ethyl methanesulfonate as a brown oil (63.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06664265B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-1cacdf7ca75a4498930c5d815a234774 |
| Source note | uspto-grants-2003_12 |