HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19087511, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 19753738 | HCID 19753738 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 19087511 | HCID 19087511 | 90% |
Reaction Steps
While cooled and stirred, 5.4 g of phosphorus oxychloride were added dropwise to 11.0 g of dimethylformamide, and 3.7 g of N,N'-di-n-butyl-N,N'-diphenyl-1, 5-diaminopentane dissolved in dimethylformamide were added dropwise to the resulting solution, followed by heating and stirring at 85° C. for 2.5 hours. After the completion of the reaction, sodium acetate, water and ethyl acetate were added to the reaction solution to separate an ethyl acetate layer, which was in turn concentrated. The concentrate was purified through a column with a mixed solvent of ethyl acetate with n-hexane to obtain 3.8 g of N,N'-di-n-butyl-N,N'-bis-(4-formylphenyl)-1,5-diaminopentane in a 90% yield (which was found to have a melting point 51°-52° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05304528 |
| Source dataset | uspto-grants-1994_04 |
| ORD ID | ord-f9e686a5943e4e4e930e30eeb85d8603 |
| Source note | uspto-grants-1994_04 |