HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86663416, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 86663414 | HCID 86663414 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86663416 | HCID 86663416 | 90.4% |
Reaction Steps
Methanesulfonyl chloride (26 mL, 0.336 mol) was added dropwise to a solution of the compound (102.11 g, 0.226 mol) obtained in Example 1c, triethylamine (63 mL, 0.452 mol) and 4-(dimethylamino)pyridine (2.76 g, 0.0273 mol) in dichloromethane (1000 mL) under ice cooling, and the mixture was stirred under ice cooling for 1 hour. The reaction mixture was washed with water and saturated sodium chloride solution, dried with anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-n-hexane, 30%→50%) to give the title compound (108.21 g; yield, 90%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476253B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-83c156e6cfc243309f68babe1d529af5 |
| Source note | uspto-grants-2013_07 |