HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 1-(4-chlorophenyl)-1,3-Propanediol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl 3-(4-chlorophenyl)-3-oxopropanoate | HCID 101336 | — |
| Reactant | Diisopropylaluminium hydride | HCID 21896610 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(4-chlorophenyl)-1,3-Propanediol | HCID 10330082 | 59.5% |
Reaction Steps
To a solution of 5.0 g of ethyl-4-chlorobenzoylacetate in 100 ml of methylene chloride cooled to -30° C., 77.3 ml of diisopropylaluminium hydride (1.0 mol/l toluene solution) was added, and the resulting mixture was stirred for 30 minutes and then brought back to room temperature over 3 hours, and 4.14 g of methanol and 24.3 g of water were added carefully, and the mixture was stirred for another 1.5 hours. The precipitate was filtered off, and the filtrate was concentrated. The resulting residue was purified by silica gel column chromatography (eluent; n-hexane/ethyl acetate=1/1), to obtain 2.45 g of the title compound as a pale yellow oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05856327 |
| Source dataset | uspto-grants-1999_01 |
| ORD ID | ord-bbbe2d4035484addbe187122e4fa8725 |
| Source note | uspto-grants-1999_01 |