Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 1,1'-Ethylenebis[2,5-dimethylpyrrole] | HCID 237950 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 14235034 | HCID 14235034 | — |
Reaction Steps
8.7 ml (0.093 mol) of phosphorus oxychloride are slowly added dropwise to 7.2 ml (0.093 mol) of anhydrous dimethylformamide at 0° C. The mixture is stirred at 10° C. for 15 minutes, 10 ml of 1,2-dichloroethane are added, and 10 g (0.046 mol) of 1,2-di-(2,5-dimethyl-pyrrol-1-yl)-ethane in 40 ml of 1,2-dichloroethane are added dropwise at 5° C. After a reaction time of 15 hours at room temperature, 100 g of sodium acetate in 150 ml of water are added, the mixture is heated under reflux for 5 minutes, methylene chloride is added, the phases are separated, the organic phase is concentrated and the residue is recrystallized from isopropanol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05043348 |
|---|
| Source dataset | uspto-grants-1991_08 |
|---|
| ORD ID | ord-cca6015bb80945b1a20f4f13198ee30d |
|---|
| Source note | uspto-grants-1991_08 |
|---|
