HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazinecarboxaldehyde → 4-(1-Phenyl-1-(2-formylhydrazinocarbonyl)-methylene)piperidine-1-carboxylic Acid Tert-Butyl Ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazinecarboxaldehyde | HCID 12229 | — |
| Reactant | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 4-(1-Phenyl-1-carboxy-methylene)piperidine-1-carboxylic acid tert-butyl ester | HCID 67046454 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-(1-Phenyl-1-(2-formylhydrazinocarbonyl)-methylene)piperidine-1-carboxylic Acid Tert-Butyl Ester | HCID 67046375 | 124.4% |
Reaction Steps
A mixture of 4-(1-phenyl-1-carboxy-methylene)piperidine-1-carboxylic acid tert-butyl ester (1.05 g, 3.31 mmol), EDCI (0.888 g, 4.63 mmol) and HOBt (0.626 g, 4.63 mmol) in DMF (4 mL) was stirred for 30 min at room temperature and then formic hydrazide (3.97 g, 66.2 mmol) was added. Stirring was continued for 1 h and then the mixture was poured into water and extracted with EtOAc (×3). The combined organic layers were washed (H2O ×3, brine), dried (Na2SO4) and evaporated to give the title compound (1.48 g, 97%) as a colorless oil:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07915283B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-51f5632f9ffd46df90c341a04902c401 |
| Source note | uspto-grants-2011_03 |