HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 12044043, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-(Chloromethyl)benzonitrile | HCID 70127 | — |
| Reactant | HCID 8321444 | HCID 8321444 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12044043 | HCID 12044043 | 54.3% |
Reaction Steps
In THF (8 ml) and DMF (2 ml) was dissolved 4-(naphthalene-2-sulfonyl)-2-piperazinone (290 mg), and to the mixture was added sodium hydride (60% in oil, 40 mg) at 0° C. The mixture was stirred for 20 minutes, to which was added 4-cyanobenzylchloride (182 mg), and the mixture was stirred at room temperature overnight. The reaction solution was concentrated under reduced pressure. To the residue was added water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried (MgSO4) and concentrated. The residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:2) to give colorless crystals of the title compound (220 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06403595B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-9e70e4a7492542d08bf84e3b68edc2cf |
| Source note | uspto-grants-2002_06 |