HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 18332987, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | alpha-Bromo-2-nitrotoluene | HCID 77569 | — |
| Reactant | 3-Carbethoxy-2-piperidone | HCID 97773 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18332987 | HCID 18332987 | 81.6% |
Reaction Steps
Sodium hydride (60% dispersion in oil, 2.45 g) was added to ethanol (100 ml), to which was added 3-carboethoxy-2-piperidone (10.0 g). The reaction mixture was stirred for 15 minutes, to which was added 2-nitrobenzyl bromide (13.2 g) at room temperature. The reaction mixture was stirred at 60° C. for 3 hours. Water was added to the reaction mixture, which was concentrated. The residue was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried and concentrated. The obtained crude crystals were recrystallized from ethyl acetate-hexane to give the entitled compound (14.6 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06329389B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-5d6b7880a5f6456c8ce13d06b61535fd |
| Source note | uspto-grants-2001_12 |