HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Thiophenecarbonyl chloride → HCID 13532781, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Thiophenecarbonyl chloride | HCID 78928 | — |
| Reactant | HCID 13532751 | HCID 13532751 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 13532781 | HCID 13532781 | 76.5% |
Reaction Steps
To a mixture of 1,2-bis(4-hydroxymethyl-3,5-dioxopiperazin-1-yl)ethane (6.30 g, 22 m mol) and pyridine (60 ml), thenoyl chloride (6.45 g, 44 m mol) was added gradually at 0° C., and then the mixture was stirred for 4 hours at room temperature. The solvent was removed from the reaction mixture under reduced pressure, and the residue was extracted with chloroform. The extract solution was washed with 10% sulfuric acid solution and successively with water, and was dried over magnesium sulfate. The residue obtained by removing the solvent from the extract solution under reduced pressure was purified by silica gel column chromatography (ethyl acetate, Rf value=0.6) to give the titled compound (8.20 g; yield 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04650799 |
| Source dataset | uspto-grants-1987_03 |
| ORD ID | ord-c986b45709c54c389dae100483c671f3 |
| Source note | uspto-grants-1987_03 |