HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 54230349, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Hydrazinecarboxylic acid, ethyl ester | HCID 20064 | — |
| Reactant | 1-Pentanone, 1-(4-pyridyl)- | HCID 74344 | — |
| Catalyst | p-Toluenesulfonic acid | HCID 6101 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 54230349 | HCID 54230349 | 54% |
Reaction Steps
A mixture of 8.3 gm (0.055 mole) of n-butyl 4-pyridyl ketone, 6.1 gm (0.059 mole) of ethyl carbazate and 150 ml of absolute ethanol is refluxed 17 hr. A Tlc (3% MeOH/CH2Cl2 on Silica gel) shows 50% starting material remaining. p-Toluenesulfonic acid (0.3 gm) is added and the reaction mixture refluxed 17 hr more. Tlc shows no remaining starting materials. The reaction is concentrated in vacuo. The residue is slurried with water and the solid collected, washed with water and dried. Crystallization yields 7.41 gm of the title compound having a melting point of 102.1° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05011932 |
| Source dataset | uspto-grants-1991_04 |
| ORD ID | ord-b80ab66bd86d4683a0b09c6ac972c5de |
| Source note | uspto-grants-1991_04 |