HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitroethane → HCID 1809354, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitroethane | HCID 6587 | — |
| Reactant | 4-Chlorobenzaldehyde | HCID 7726 | — |
| Reactant | Piperidine | HCID 8082 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 1809354 | HCID 1809354 | 58% |
Reaction Steps
A solution of 4-chlorobenzaldehyde (28.57 g, 203 mmol), nitroethane (44.0 mL, 610 mmol) and piperidine (4.01 mL, 40.6 mmol) in toluene (200 mL) was stirred at reflux (Dean-Stark) for 6 h and the mixture was stored at room temperature overnight. The solvent was removed under reduced pressure and the product was recrystallised from absolute EtOH. The crystals were filtered off, washed with a small amount of absolute EtOH and dried to give 23.25 g of the desired product. The mother liquor was concentrated, heated, cooled. Another batch of crystals was filtered off, washed with a small amount of absolute EtOH and dried in vacuo, to afford 3.95 g of the desired product. Total yield: 27.20 g (68%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09302988B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-a256433fda4945b493513065ac3b801e |
| Source note | uspto-grants-2016_04 |