HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2-Dimethyl-1,3-dioxane-4,6-dione → HCID 58110062, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| Reactant | HCID 86649924 | HCID 86649924 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58110062 | HCID 58110062 | 93.2% |
Reaction Steps
Step AAH (3): To a soln of 2,2-dimethyl-1,3-dioxane-4,6-dione (329 mg, 2.281 mmol) in dichloromethane (10 mL) was added DMAP (405 mg, 3.32 mmol). After stirring for 10 min, a solution of 4-(2-phenyl-1,3-dioxolan-2-yl)butanoyl chloride (2.07 mmol) in dichloromethane was added at 0° C. under nitrogen. The mixture was stirred at rt for 3 his. The crude reaction mixture was concentrated in vacuo. The residue was dissolved in EtOAc. The organic layer was sequentially washed with 1.0 N aqueous HCl, 1.0 N aqueous NaOH, and water. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo to 2,2-dimethyl-5-(4-(2-phenyl-1,3-dioxolan-2-yl)butanoyl)-1,3-dioxane-4,6-dione (700 mg, 1.93 mmol, 93% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08349880B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-ab8ce1b6cb0f4a75a5c980b7cd01ab74 |
| Source note | uspto-grants-2013_01 |