HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 11663113, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Reactant | HCID 11696573 | HCID 11696573 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11663113 | HCID 11663113 | — |
Reaction Steps
To a stirred solution of the compound from example 5 (270 mg, 0.71 mmol) in dichloromethane (20 mL) was added triethylamine (118.8 μL, 0.86 mmol) followed by dimethylsulfamoyl chloride (84 μL, 0.78 mmol) and the reaction mixture was stirred for 16 hours. Dimethylsulfamoyl chloride (84 μL, 0.78 mmol) was then added and the reaction stirred for a further 72 hours. The reaction was diluted with water (20 mL) and the phases separated. The organic phase was washed with brine, dried over magnesium sulfate and concentrated in vacuo to give the crude residue. Purification by column chromatography on silica gel using ethyl acetate and then dichloromethane methanol (95:5) as eluent gave the product as a white crystalline solid, 217 mg (63%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07456170B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-7294e6c347224daa81100eb20384f873 |
| Source note | uspto-grants-2008_11 |