HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2-Dimethyl-1,3-dioxane-4,6-dione → HCID 67318079, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| Reactant | Ethyl orthoformate | HCID 31214 | — |
| Reactant | 3,5-Difluoroaniline | HCID 96595 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 67318079 | HCID 67318079 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
In a oven dried 2-neck RBF equipped with reflux condenser and inert atmosphere, meldrum's acid (30 g, 0.208 mole) was dissolved in triethylorthoformate (185 g, 1.25 mole) and the reaction mixture was refluxed at 100° C. under nitrogen for 1 h. On complete consumption of starting material (tic), 3,5-difluoroaniline (26.8 g, 0.208 mol) was added and the heating continued for 4 h. After completion of the reaction (tic), reaction mixture was brought to RT and diluted with hexane (300 ml) when yellow solid precipitated. The solid was filtered, washed thoroughly with hexane and dried to furnish the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557816B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-39d7d716812d4a6cb8fb795fc391d72c |
| Source note | uspto-grants-2013_10 |