HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 57850366, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 24729731 | HCID 24729731 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57850366 | HCID 57850366 | 62.4% |
Reaction Steps
To a solution of [3-hydroxy-1-(tetrahydro-pyran-4-yl)-propyl]-carbamic acid tert-butyl ester (0.200 g, 0.770 mmol) and NEt3 (192 μL, 0.920 mmol) in CH2Cl2 (8 mL) was added MsCl (72 μL, 0.92 mmol) at 0° C. and the mixture was stirred at room temperature for 10 h. The solvent was evaporated to dryness and EtOAC was added. The ethyl acetate layer was washed with aq. NaHCO3, dried (Na2SO4), filtered, and solvent was evaporated under reduced pressure to afford methanesulfonic acid 3-tert-butoxycarbonylamino-3-(tetrahydro-pyran-4-yl)-propyl ester (0.162 g). LC-MS [M+Na] 360.2. The product was sufficiently pure for the next step and used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476285B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-2dc8def7818046cab7b49bac1ce4c475 |
| Source note | uspto-grants-2013_07 |