Acetonitrile → HCID 70357837、化合物
反応式
[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6](CCl)=[CH:7]2.[C-]#N.[Na+].[CH3:17][C:18]#[N:19]>O>[Cl:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[C:7]2[CH2:17][C:18]#[N:19]参加物
5
実験手順
A mixture of 5-chloro-2-chloromethylnaphthalene (1.37 g crude product, 5.12 mmol), NaCN (0.275 g, 5.61 mmol), CH3CN (10 mL), and H2O (1 mL) was heated under reflux for 5.5 hours, cooled, and stirred at room temperature overnight. The mixture was partitioned between ether and H2O. The aqueous phase was extracted with ether, and the combined ether layers were washed with brine, dried (MgSO4), and concentrated in vacuo. Purification by flash chromatography (eluant EtOAc/hexane (10:90)) gave a pale yellow solid (600 mg, 58%), m.p. 95°-98° C.
後処理
- temperaturewas heated
- temperatureunder reflux for 5.5 hours
- temperaturecooled
- customThe mixture was partitioned between ether and H2O
- extractionThe aqueous phase was extracted with ether
- washthe combined ether layers were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customPurification by flash chromatography (eluant EtOAc/hexane (10:90))
出典と根拠
- ORDレコード
- ord-11511cca37b04c73aa9309da00af4934
- 出典データセット
- uspto-grants-1990_01
- 特許番号
- US04897405
反応ノート
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