HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 13457764, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 13457763 | HCID 13457763 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 13457764 | HCID 13457764 | 90.4% |
Reaction Steps
To a stirred slurry containing 1-amino-2-(2-chlorobenzoyl)-5-methylpyrrole (27.1 g, 0.115 mol) and sodium bicarbonate (16.8 g, 0.20 mol) in 300 ml of dichloromethane was added ethyl chloroformate (21.7 g, 0.20 mol) over 5 minutes. The reaction mixture was stirred at room temperature overnight and thereafter quenched with 500 ml of H2O. The organic layer was washed with brine, dried (MgSO4), charcoaled, filtered, and evaporated to an oil. This oil crystallized in hexane, which was recrystallized from ether-hexane to give 31.9 g (90%) of powder, m.p. 82°-84°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04588727 |
| Source dataset | uspto-grants-1986_05 |
| ORD ID | ord-1e4440b56f374edb9474d95ebb9e4c89 |
| Source note | uspto-grants-1986_05 |