HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → N2 (benzyloxycarbonyl)-N1-tert.butyl-4(S)-(methanesulphonyloxy)-L-prolinamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | N2 (benzyloxycarbonyl)-N1-tert.butyl-4(S)-hydroxy-L-prolinamide | HCID 86746280 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | N2 (benzyloxycarbonyl)-N1-tert.butyl-4(S)-(methanesulphonyloxy)-L-prolinamide | HCID 86746278 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
0.32 g of N2 -(benzyloxycarbonyl)-N1 -tert.butyl-4(S)-hydroxy-L-prolinamide was dissolved in 5 ml of dry pyridine while stirring, cooled to 0° C. and treated dropwise with 0.82 ml of methanesulphonyl chloride. The solution was stirred at 0° C. for a further 2 hours. The mixture was poured into a mixture of ice and water which was then extracted with ethyl acetate. The combined organic extracts were washed with 2M hydrochloric acid and then with saturated sodium bicarbonate solution and subsequently dried over anhydrous sodium sulphate. After evaporation there was obtained 0.5 g of N2 -(benzyloxycarbonyl)-N1 -tert.butyl-4(S)-(methanesulphonyloxy)-L-prolinamide as an oil which was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05554756 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-fa12c56049fe400e864349b2f0e35d15 |
| Source note | uspto-grants-1996_09 |