HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59361434, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 46194242 | HCID 46194242 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59361434 | HCID 59361434 | 18.3% |
Reaction Steps
Under an argon atmosphere, a solution of 1-(4-aminophenyl)-4,4-dimethyl-2-(adamantan-2-yl)-1,2-diazetidin-3-one (30.0 mg, 0.0920 mmol) prepared in Example 183 in dichloromethane (1 mL) was added with triethylamine (18.6 mg, 0.184 mmol) and methanesulfonyl chloride (15.8 mg, 0.138 mmol) at room temperature, and the resultant was stirred at the same temperature for 3 hours. The reaction solution was added with water and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo, the obtained residue was purified using Preparative Thin-Layer chromatography (hexane:ethyl acetate=1:1), and the title compound (6.80 mg, 18.3%) was obtained as a brown amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08252781B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-eba04509cab14dce879b7704de01fe24 |
| Source note | uspto-grants-2012_08 |