HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 59443012, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2,5-Hexanedione | HCID 8035 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | 3-Chloro-5-fluoroaniline | HCID 2734838 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 59443012 | HCID 59443012 | — |
Reaction Steps
2,5-Hexanedione (4.51 mL) and p-toluenesulfonic acid monohydrate (73 mg) were added to a solution of 3-chloro-5-fluoroaniline (5.12 g) in toluene (40 mL)-tetrahydrofuran (40 mL), and the mixture was heated under reflux for 3.5 hours. After being cooled down, the reaction solution was concentrated in vacuo, and the resultant residue was dissolved in chloroform. The solution was washed successively with water and brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The resulted residue was purified by column chromatography on silica gel (Solvent: n-hexane/ethyl acetate=97/3) to give the titled compound (7.63 g) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08258131B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-ea84b074c18a48daab804fd57cd92c54 |
| Source note | uspto-grants-2012_09 |