HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 9948737, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sodium ethoxide | HCID 2723922 | — |
| Reactant | HCID 12993786 | HCID 12993786 | — |
| Product | HCID 9948737 | HCID 9948737 | — |
Reaction Steps
0.11 g of 6-methyl-5-(3-methylisoxazol-5-yl)-1,2,3,4-tetrachlorobicyclo[2.2.1]hept-2en-7-one (a mixture of trans:cis=1:1) was dissolved in 1 ml of ethanol, and 0.06 g of sodium ethylate was added, while cooling with ice. The resulting solution was stirred for an hour at room temperature. The reaction solution was poured into 50 ml of ice-water, and extracted with 30 ml of ethyl acetate twice. The organic layer was washed with saturated salt water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The obtained viscous liquid was purified on silica gel column chromatography (elution with n-hexane/ethyl acetate) to give 0.024 g of the title compound as white crystals. Melting point 86-88° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06756497B1 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-2475cc011f924869915d7243da40fe20 |
| Source note | uspto-grants-2004_06 |