HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86615896, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 59771240 | HCID 59771240 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86615896 | HCID 86615896 | — |
Reaction Steps
To a suspension of [4-(2-hydroxy-1-hydroxymethyl-ethyl)-phenyl]-carbamic acid tert-butyl ester (267 mg, 1.00 mmol, as prepared in the previous step) in DCM (10 mL) and Et3N (0.35 mL, 2.5 mmol), methanesulfonyl chloride (MsCl) (0.15 mL, 2.0 mmol) was added dropwise at 0° C. The resulting mixture was stirred at RT for 30 min, diluted with DCM (10 mL) and washed with satd NaHCO3 (20 mL). The organic layer was separated, dried (Na2SO4) and concentrated to afford methanesulfonic acid 2-(4-tert-butoxycarbonylamino-phenyl)-3-methanesulfonyloxy-propyl ester, which was dried in vacuo and directly used in next step: Mass spectrum, (ESI, m/z): Calcd. for C16H25NO8S2, 446.1 (M+Na). found 446.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08759347B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-81a8be1db9cd4068870a6baba1603523 |
| Source note | uspto-grants-2014_06 |