HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22607842, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Isomaltol | HCID 18898 | — |
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22607842 | HCID 22607842 | — |
Reaction Steps
Isomaltol (6.3 g, 0.05 moles) in 60 ml of CH2Cl2 was added dropwise over 10 minutes to a solution of PCl5 (10.4 g, 0.05 moles) in 125 ml of CH2Cl2 at 4° C. After stirring at 4°-5° C. for 1 hour, the reaction was allowed to come to room temperature, poured into 350 ml of water and the CH2Cl2 layer separated. The aqueous layer was then extracted with CH2Cl2, the CH2Cl2 layers combined and then concentrated to yield a dark oil, 7.0 g. Pure 2-acetyl-3-chloro-furan was obtained by chromatography from silica gel, NMR (CDCl3, δ) 7.5 (1H, d, J=2Hz), 6.56 (1H, d, J=2Hz), 2.53 (3H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04173572 |
| Source dataset | uspto-grants-1979_11 |
| ORD ID | ord-0ef49ee81cee40e2bf8c44ec76e31cea |
| Source note | uspto-grants-1979_11 |