HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → Dimethyl 4-[2-(acetylthio)ethyl]-1,3-benzenedicarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | Dimethyl 4-ethenyl-1,3-benzenedicarboxylate | HCID 12017547 | — |
| Reactant | HCID 178418634 | HCID 178418634 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | Dimethyl 4-[2-(acetylthio)ethyl]-1,3-benzenedicarboxylate | HCID 12017548 | 27% |
Reaction Steps
To a degassed solution of dimethyl 4-ethenyl-1,3-benzenedicarboxylate (415 mg, 1.88 mmol) in benzene (6 mL) were added AIBN (33 mg, 0.21 mmol) and thioacetic acid (0.27 mL, 3.78 mmol), and the mixture was refluxed for 5 hours. The reaction mixture was diluted with aqueous NaHCO3 solution (15 mL) and extracted with EtOAc (15 mL). The organic layer was dried over MgSO4 and concentrated. The residual material was purified by silica gel chromatography (hexanes/EtOAc=10:1) to give 0.150 g of colorless oil (27% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06852750B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-2fd6baa986b74fccad2714dfe20d51dd |
| Source note | uspto-grants-2005_02 |