HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylamine → HCID 59591390, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Chlorosulfonic acid | HCID 24638 | — |
| Reactant | 3-Chloro-2-fluorobenzoic acid | HCID 302931 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59591390 | HCID 59591390 | — |
Reaction Steps
3-chloro-2-fluorobenzoic acid (200 mg, 1.146 mmol) in chlorosulfonic acid (1.535 ml, 22.92 mmol) was stirred at room temperature for 30 seconds, then microwaved at 200 degrees for 10 rains. The reaction mixture was cooled to room temperature and dumped on ice (10 g) slowly. Ethyl acetate (25 ml) was added and extracted twice with ethyl acetate (10 mL X2). The combined organic phase was dried over MgSO4. Ethylamine (1833 μl, 3.67 mmol) in THF (2.0 M) was added, stirred at room temperature for 10 mins and washed with 1 N HCl (10 ml). The organic phase was dried over MgSO4 and concentrated to give the title compound, which was carried the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08044075B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-6563ce5547464d80912a31484c2baaef |
| Source note | uspto-grants-2011_10 |