HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropyl acetoacetate → HCID 20077494, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropyl acetoacetate | HCID 68329 | — |
| Reactant | (2Z)-3-Amino-2-butenenitrile | HCID 5325263 | — |
| Reactant | HCID 20077497 | HCID 20077497 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 20077494 | HCID 20077494 | 23.6% |
Reaction Steps
750 mg (3.2 mmol) of 3-phenyl-5-cinnolinecarboxaldehyde, 263 mg (3.2 mmol) of 3-aminocrotononitrile and 457 mg (3.2 mmol) of isopropyl acetoacetate are boiled under reflux for 2.5 days in 25 ml of ethanol. The mixture is concentrated and separated on a silica gel column using toluene/ethyl acetate mixtures. The desired fractions are collected and concentrated. The evaporation residue obtained is crystallised using ether and filtered off with suction. 320 mg of crystals of melting point 200°-202° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05364855 |
| Source dataset | uspto-grants-1994_11 |
| ORD ID | ord-948d04af4be14806a7c4e331696a0554 |
| Source note | uspto-grants-1994_11 |