HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 131722890, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Reactant | HCID 86584131 | HCID 86584131 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131722890 | HCID 131722890 | 46% |
Reaction Steps
A solution of 0.5 g (1.5 mmol) of material from Example 28, Step B and 0.52 mL (3.70 mmol) of triethylamine in 10 mL of dichloromethane was cooled to 0° C. A solution of 0.16 mL (1.5 mmol) of dimethylsulfamoyl chloride in 1 mL of dichloro-methane was added dropwise. The ice-bath was removed and the mixture was stirred at ambient temperature for 5 h. The mixture was washed with 10 mL of 10% aqueous sodium bisulfate, the organic layer was separated and the aqueous layer extracted three times with 5 mL of dichloromethane. The combined organics were dried (MgSO4), filtered and concentrated in vacuo. The residue was suspended in 50% ether/hexane and filtered to afford 0.22 g (46%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06596716B2 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-d1de831646b0448fa9b50515b2d60423 |
| Source note | uspto-grants-2003_07 |