HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 89862352, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 65916912 | HCID 65916912 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89862352 | HCID 89862352 | 97% |
Reaction Steps
To a solution of Intermediate 3A (1.87 g, 6.19 mmol) and Et3N (1.724 mL, 12.37 mmol) in DCM (30 mL) was added a solution of methanesulfonyl chloride (0.53 mL, 6.8 mmol) in DCM (10 mL) over 1 h at rt. The reaction mixture was stirred at rt for 2.5 h. Additional Et3N (1.724 mL, 12.37 mmol) and methanesulfonyl chloride (0.53 mL, 6.8 mmol) were added and stirred for another 1 h. The reaction mixture was partitioned between 1 N HCl and DCM. The organic layer was dried over Na2SO4, filtered and the solvent was evaporated under reduced pressure to give Intermediate 3B (1.7 g, 5.9 mmol, 97% yield). LC-MS (ESI) m/z 285 (M+H), RT=3.43 min (Method C).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09199946B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-577c20b990f64f279ed7d0af1cd48868 |
| Source note | uspto-grants-2015_12 |