HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 86702738, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Malononitrile | HCID 8010 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 67516257 | HCID 67516257 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86702738 | HCID 86702738 | — |
Reaction Steps
0.500 g (1.70 mmol) of 2-(2,6-diethyl-4-methylphenyl)tetrahydropentalene-1,3,5-trione (example I-a-4 from WO 2010/040460), 250 mg of malononitrile, 150 mg of ammonium acetate and 0.3 ml of glacial acetic acid in 30 ml of toluene are heated at reflux for 2 h. After cooling, the solvent is distilled off and the mixture is taken up in ethyl acetate, washed twice with water, then dried (magnesium sulphate) and concentrated on a rotary evaporator. What remains is a yellow oil which is chromatographed on silica gel using ethyl acetate/hexane 1:6. This gives 0.32 g (56%) of a colourless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09101133B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-419d9fcfecb44f818a9d889845f24c54 |
| Source note | uspto-grants-2015_08 |