HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 178452384, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 5-oxo-1-phenyl-2,5-dihydro-1H-pyrazole-3-carboxylic acid | HCID 9167391 | — |
| Reactant | HCID 66713063 | HCID 66713063 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Diisopropylethylamine | HCID 81531 | — |
| Product | HCID 178452384 | HCID 178452384 | — |
Reaction Steps
To a solution of 2.77 g of 1-phenyl-3-carboxy-5-pyrazolone and 3.3 g 4-(2-Amino-acetyl)-piperazine-1-carboxylic acid butyl ester in 70 ml DMF 2.7 g HOBT, 5.6 ml DIPEA and 3.4 g EDC were added and the reaction mixture was stirred for 12 h at RT. Then the reaction mixture was diluted with ethyl acetate and subsequently extracted with aqueous LiCl (4% w/w), 0.1 M HCl and aqueous NaHCO3. The organic layer was dried over MgSO4 and the solvent was removed under reduced pressure. The crude product thus obtained was used in the subsequent reaction. Yield: 5.3 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08426420B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-285de2842da74d3693cadef7007691fd |
| Source note | uspto-grants-2013_04 |