HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → N-cyano-N'-[2-(2,2-dichloro-3-oxobutylthio)]ethyl-N"-methylguanidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | N-[2-(2-chloro-3-oxobutylthio)ethyl]-N'-cyano-N"-methylguanidine | HCID 14153741 | — |
| Reactant | Sodium Hypochlorite | HCID 23665760 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | N-cyano-N'-[2-(2,2-dichloro-3-oxobutylthio)]ethyl-N"-methylguanidine | HCID 14622765 | 25% |
Reaction Steps
In 1 ml of methanol was dissolved 131 mg of N-[2-(2-chloro-3-oxobutylthio)]ethyl-N'-cyano-N"-methylguanidine, and 0.63 ml of an aqueous solution of sodium hypochlorite was added to the solution and reaction was carried out at room temperature for 3 hours. Then, 15 ml of ethyl acetate was added to the reaction liquid and the organic layer was recovered. The obtained organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was refined by silica gel column chromatography (developing solvent: ethyl/ethanol=10/1) to obtain 37 mg of a colorless oily product (the yield was 25%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04886912 |
| Source dataset | uspto-grants-1989_12 |
| ORD ID | ord-959a54c27c094801bf58b2dfebe9a1fd |
| Source note | uspto-grants-1989_12 |