HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-[(3-Methoxyphenylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione → HCID 178487715, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-[(3-Methoxyphenylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 757248 | — |
| Solvent | Diphenyl Ether | HCID 7583 | — |
| Product | HCID 178487715 | HCID 178487715 | 45.1% |
Reaction Steps
5-{[(3-Methoxyphenyl)amino]methylene}-2,2-dimethyl-1,3-dioxane-4,6-dione (Intermediate 11, 43.5 g, 157 mmol) was added in small portions to phenylether (200 mL) at 225-260° C. under stirring. The reaction mixture was stirred for an additional 5 minutes, until the evolution of gas had stopped. The reaction mixture was cooled to room temperature and the precipitate was collected by filtration and washed with hexanes. Purification by recrystallization from methanol gave 12.4 g (45% yield) of product as a green solid, mp 210° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07875715B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-502faa50ae6944dfaed900016a46a967 |
| Source note | uspto-grants-2011_01 |