HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19972408, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | HCID 19972408 | HCID 19972408 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 19972408 | HCID 19972408 | — |
| Product | HCID 19972532 | HCID 19972532 | — |
Reaction Steps
A solution of 2.5 g of Intermediate XIX in 25 ml of xylene and 3 ml of dioxane was prepared. 0.15 g of sodium was dissolved in 3.10 ml of anhydrous ethylene glycol, and this solution was added dropwise at ambient temperature to the solution of Intermediate XIX. After refluxing for 5.5 hours, the reaction mixture was cooled to ambient temperature and poured into 50 ml of water. It was extracted with dichloromethane, and the extract was washed with sodium chloride solution, dried on anhydrous sodium sulfate and evaporated to dryness in vacuo. The solid residue was crystallized from ethanol, giving 2.1 g of the title compound, m.p. 132°-133° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05605896 |
| Source dataset | uspto-grants-1997_02 |
| ORD ID | ord-ff9124022ea64cc2a4d6d3cf1807abdb |
| Source note | uspto-grants-1997_02 |