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 | 100% |
Reaction Steps
Under a nitrogen atmosphere, a solution of tert-butyl 2-(2-hydroxyethoxy)ethylcarbamate (48.53 g, 236 mmol) in anhydrous dichloromethane (1 L) was cooled to 0° C. Triethylamine (49.4 mL, 354 mmol)) was added. Methanesulfonyl chloride (20.10 mL, 260 mmol) was added dropwise over a period of 10 minutes. The reaction was allowed to warm to ambient temperature and stir overnight. The reaction was quenched with saturated sodium bicarbonate solution (500 mL). The organic layer was washed with water (3×500 mL) and brine (1×500 mL), dried over sodium sulfate and then concentrated under reduced pressure to provide 66.9 g of 2-{2-[(tert-butoxycarbonyl)amino]ethoxy}ethyl methanesulfonate as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08168802B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-b15331b450ff45689e174369c6a4a46e |
| Source note | uspto-grants-2012_05 |