Acetonitrile → HCID 70357837, 화합물
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- 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))
출처 및 근거
- ORD 기록
- ord-541ea265c77d4ed883f70548f611c58a
- 출처 데이터셋
- uspto-grants-1990_10
- 특허 번호
- US04966975
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