HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 86731704, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Carbamic acid, N-[2-ethoxy-1-(hydroxymethyl)ethyl]-, 1,1-dimethylethyl ester | HCID 75089283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86731704 | HCID 86731704 | — |
Reaction Steps
To a solution of tert-butyl (1-ethoxy-3-hydroxypropan-2-yl)carbamate (2.2 g, 9.4 mmol) in DCM (40 mL) was added methanesulfonylchloride (2.10 g, 18.8 mmol) at 0° C. The reaction mixture was allowed to warm to ambient temperature. After 12 hours, the reaction mixture was concentrated under reduced pressure. The residue was purified via chromatography on silica gel to afford 2-[(tert-butoxycarbonyl)amino]-3-ethoxypropyl methanesulfonate. MS ESI calc'd. for C11H24NO6S [M+H]+ 298. found 298. 1H NMR (400 MHz, CDCl3) δ 4.95 (s, 1H), 4.28 (d, J=8.0 Hz, 1H), 4.13-4.11 (m, 1H), 3.58-3.48 (m, 5H), 3.03 (s, 3H), 1.45 (s, 9H), 1.18 (t, J=6.8 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09216173B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-ef680de5d5d0468c9575847a2f2e194b |
| Source note | uspto-grants-2015_12 |