HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 87485559, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl nitroacetate | HCID 69379 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | (3E)-6-Methyl-3-hepten-2-one | HCID 5462986 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 87485559 | HCID 87485559 | — |
Reaction Steps
Diisopropylethylamine (7.9 mL) was added to the acetonitrile solution (50 mL) of (3E)-6-methylhept-3-en-2-one (6.25 g) and nitro ethyl acetate (5 mL) under argon gas atmosphere, and the reaction mixture was stirred at room temperature overnight. 1N hydrochloric acid was added to the reaction mixture, and the reaction mixture was extracted with ethyl acetate. The organic layer was washed by water and a saturated aqueous solution of sodium chloride, and dried with anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=95/5→75/25) to obtain the title compound (9.88 g) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08420810B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-c314685cc1e749a1b5ad6d686abe61d9 |
| Source note | uspto-grants-2013_04 |