HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2-Dimethyl-1,3-dioxane-4,6-dione → HCID 17138478, 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-Benzyloxyaniline | HCID 92892 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 17138478 | HCID 17138478 | 98.2% |
Reaction Steps
To a solution of 3-(Benzyloxy)benzenamine (970 g, 4.9 mol, Wuhan Xinghuayuan Tech. Co. Ltd.) and 2,2-dimethyl-1,3-dioxane-4,6-dione (842.3 g, 5.8 mol) in anhydrous EtOH (970 mL) was added triethoxymethane (865.7 g, 5.8 mol). The suspension was heated to reflux for 1 hour. The reaction mixture was then cooled to room temperature, and continued to stir for additional 2 hours. The suspension was filtered, and the solid was stirred in anhydrous EtOH (970 mL) for 2 hours, collected by filtration. The solid was dried in vacuo at 45° C. to give the title compound as a pale yellow solid (1.7 kg, 96.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133162B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-756f663b80504a1d949cf6d17835ed08 |
| Source note | uspto-grants-2015_09 |