HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 131733023, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ethyl cyanoacetate | HCID 7764 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 3,3-Dimethylcyclopentan-1-one | HCID 643102 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 131733023 | HCID 131733023 | — |
Reaction Steps
To a round bottomed flask equipped with a stir bar, reflux condenser, and Dean Stark trap were added 3,3-dimethylcyclopentanone (3.4 g, 30 mmol), toluene (50 mL), and ethyl 2-cyanoacetate (3.4 g, 30 mmol), ammonium chloride (231 mg, 3 mmol) and acetic acid (0.36 mL, 6 mmol). The reaction mixture was refluxed for 24 h. The reaction was cooled to RT and concentrated to dryness. The residue was diluted with water (100 mL) and extracted with ethyl acetate (2×100 mL). The combined organic phases were dried with Na2SO4, concentrated to dryness subjected to FCC to afford the title compound as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09265770B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-341b1e11879b4f2688d1732753dd3aec |
| Source note | uspto-grants-2016_02 |