HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → [2,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxin-6-yl]methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 23332965 | HCID 23332965 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | [2,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxin-6-yl]methanol | HCID 23332968 | — |
Reaction Steps
A solution of ethyl 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylate (2.0 g.) in anhydrous ether (25 ml.) was added at room temperature during 20 minutes to a suspension of lithium aluminium hydride (0.2 g.) in anhydrous ether (25 ml.). The mixture was stirred for 1 hour, then ethyl acetate (5 ml.) was added, followed by water (10 ml.). The mixture was filtered, and the ether layer of the filtrate was separated. The aqueous phase was extracted with ether (3×10 ml.), the combined extracts were dried, and the solvent was evaporated. The residue was crystallised from ethanol to give 6-hydroxymethyl-2,4-bis(trichloromethyl)benzo[1,3]dioxin, m.p. 134°-136° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04232032 |
| Source dataset | uspto-grants-1980_11 |
| ORD ID | ord-cb836e190bc84a4ebd3aa1b1f8198efb |
| Source note | uspto-grants-1980_11 |