HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (2S)-2-[(tert-butoxycarbonyl)amino]-2-phenylethyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | (S)-2-((N-tert-Butoxycarbonyl)amino)-2-phenylethanol | HCID 7016462 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (2S)-2-[(tert-butoxycarbonyl)amino]-2-phenylethyl methanesulfonate | HCID 10335849 | 98% |
Reaction Steps
The solution of 68.9 g (0.29 mol) of tert-butyl (1S)-2-hydroxy-1-phenylethylcarbamate and triethylamine (40.36 mL, 0.29 mol) in 700 mL of dry dichloromethane under inert atmosphere was cooled to −10° C. and 24.79 mL (0.319 mol) of mesylchloride were added dropwise. After 2 hours at 0° C. the mixture was poured into ice and water and extracted with dichloromethane. The organic phase was washed with diluted HCl, aqueous NaHCO3, brine and dried over Na2SO4 yielding 89.8 g of the product (98% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08541429B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-13200e85ff694201877cc88e63376806 |
| Source note | uspto-grants-2013_09 |