HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86663474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 66688271 | HCID 66688271 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86663474 | HCID 86663474 | 110.5% |
Reaction Steps
The compound (1.50 g, 3.80 mmol) obtained in Example 91d was dissolved in methylene chloride (60 mL), the mixture was stirred under ice cooling, methanesulfonyl chloride (0.35 mL, 4.56 mmol) and triethylamine (0.79 mL, 5.70 mmol) were added, and the mixture was stirred at the same temperature under a nitrogen atmosphere for 4 hours. After the reaction was completed, water was added to the reaction mixture under ice cooling, and ethyl acetate was further added to separate the layers. The resulting organic layer was separated, washed with saturated sodium chloride solution, and then dried with anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give a crude title compound (1.98 g) as a colorless oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476253B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-fcd50cb4525646fda217b313c6703241 |
| Source note | uspto-grants-2013_07 |