HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → 2-Cyclohexyl-8-ethenesulfonyl-1,3,8-triaza-spiro[4.5]dec-1-en-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| Reactant | 2-Cyclohexyl-1,3,8-triaza-spiro[4.5]dec-1-en-4-one dihydrochloride | HCID 66818102 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Cyclohexyl-8-ethenesulfonyl-1,3,8-triaza-spiro[4.5]dec-1-en-4-one | HCID 66816377 | 66% |
Reaction Steps
2-Chloro-ethanesulfonyl chloride (440 μl, 4.21 mmol) was added to a solution of 2-cyclohexyl-1,3,8-triaza-spiro[4.5]dec-1-en-4-one dihydrochloride (1.50 g, 3.24 mmol) and triethylamine (2.7 ml, 19.4 mmol) in CH2Cl2 (30 ml) at room temperature in an N2 atmosphere. The mixture was stirred at room temperature for 30 minutes, and then washed with water, dried over sodium sulfate and concentrated under reduced pressure. The resulting residue was triturated with AcOEt-hexane, and the solid was then collected by filtration and dried to give 2-cyclohexyl-8-ethenesulfonyl-1,3,8-triaza-spiro[4.5]dec-1-en-4-one as a colorless solid (692 mg, 66%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169254B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-d97f3d53c79047a893135f07a349d54f |
| Source note | uspto-grants-2015_10 |