HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 12926196, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 4-Fluorophenylhydrazine hydrochloride | HCID 69981 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12926196 | HCID 12926196 | 80.5% |
Reaction Steps
To a solution of 4-fluorophenylhydrazine hydrochloride (2 g, 12.05 mmol) in THF (60 mL) is added DIPEA (6 mL, 34.40 mmol), ethyl chloroformate (1.2 mL, 12.55 mmol) and 4-dimethylaminopyridine (0.16 g, 1.31 mmol). The mixture is stirred at RT for 4 hours. The reaction is diluted with water and extracted with EtOAc, the organic phase is washed with saturated aqueous sodium chloride, dried over Na2SO4 and concentrated. The residue is purified by column chromatography on silica gel, eluting with DCM then DCM:MeOH (80:1) to afford the title compound (1.92 g, 80.5% yield). MS (m/z): 199 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030302B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-1e9405ed13844f59b08b3d1315f41e46 |
| Source note | uspto-grants-2011_10 |