HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 58784962, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ethyl Acrylate | HCID 8821 | — |
| Reactant | Ethyl 3-acetyl-4-oxopentanoate | HCID 87820 | — |
| Catalyst | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 58784962 | HCID 58784962 | 81.2% |
Reaction Steps
37 g of 3-acetyl-4-oxo-pentanoic acid ethyl ester, synthesized according to the procedure given in Example 15, and 0.3 g of 1,8-diazabicyclo-[5.4.0]-undec-7-ene were mixed, and 30 g of ethyl acrylate was added dropwise over 30 minutes. After stirring for 24 hours, the base was neutralized by adding acetic acid. 80 ml of diethyl ether was added, and the mixture was extracted with 60 ml of an aqueous sodium carbonate solution and 150 ml of water. Fractional distillation of the water-free organic layer yielded 46.2 g of 3,3-diacetyl-hexanedioic acid diethyl ester (boiling point: 150° C./0.03 mbar; purity: >99%; colorless).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07166648B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-a4aea11dd1d44f469542f68f53bc16a6 |
| Source note | uspto-grants-2007_01 |