HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178454136, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 178454126 | HCID 178454126 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178454136 | HCID 178454136 | 102% |
Reaction Steps
A solution of tert-butyl(trans-3-hydroxycyclobutyl)carbamate (20.05 g, 107 mmol, Pharmacore) and triethylamine, anhydrous (22.34 mL, 161 mmol, Sigma-Aldrich Chemical Company, Inc.) in DCM (200 mL) was cooled to −30° C. and methanesulfonyl chloride (9.94 mL, 129 mmol, Sigma-Aldrich Chemical Company, Inc.) was added dropwise over 20 min period. The mixture was stirred at room temperature for 12 h, washed with 200 mL water, then 200 mL 10% aq. citric acid followed by brine, dried over Na2SO4 and evaporated to give the title compound (29 g, 109 mmol, 102% yield), which was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174992B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-c1bc6a11a6944eeca5ddf106b124536d |
| Source note | uspto-grants-2015_11 |