HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 21190284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 21190076 | HCID 21190076 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21190284 | HCID 21190284 | 22.4% |
Reaction Steps
To a suspension of 877 mg (3.0 mmol) of 4-[4-(amino)phenylmethyl]-4,5-dihydro-3H-1,4,8b-triazaacenaphthylene-3,5-dione and 0.63 ml (4.5 mmol) of triethylamine in methylene chloride (60 ml) was added dropwise 0.30 ml (3.9 mmol) of methanesulfonyl chloride while stirring at room temperature. The mixture was stirred for 72 hours at room temperature. The solvent was distilled off. To the residue was added chloroform, washed with 1N-HCl, and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by column chromatography (eluent: chloroform/methanol=20:1) to afford 274 mg of the desired compound (24.7%, a pale yellow solid).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05958942 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-40300b8d907a4ad482e9edf86eb75aef |
| Source note | uspto-grants-1999_09 |