Potassium Cyanide → HCID 20092979, 화합물
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Cl[C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[CH:6][N:5]=[CH:4][N:3]=1.[C-:15]#[N:16].[K+].C1OCCOCCOCCOCCOCCOC1>C(#N)C>[C:15]([C:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][CH:9]=2)=[CH:6][N:5]=[CH:4][N:3]=1)#[N:16]참가 물질
5
실험 절차
A mixture of 4-chloro-5-(p-tolyl)pyrimidine (7.4 g, 36 mmol), potassium cyanide (4.74 g, 72 mmol) and 18-crown-6 ether (0.48 g, 2 mmol) in acetonitrile (130 ml) was heated under reflux for 17 hours. After removal of insoluble materials by filtration from the reaction mixture, the filtrate was concentrated to dryness. The residue was purified by column chromatography on silica gel to give crystals. Recrystallization from ethyl acetate-hexane afforded pale yellow needles (4.17 g, 59%), m.p. 107°-109° C.
후처리
- temperaturewas heated
- temperatureunder reflux for 17 hours
- customAfter removal of insoluble materials
- filtrationby filtration from the reaction mixture
- concentrationthe filtrate was concentrated to dryness
- customThe residue was purified by column chromatography on silica gel
- customto give crystals
- customRecrystallization from ethyl acetate-hexane afforded pale yellow needles (4.17 g, 59%), m.p. 107°-109° C.
출처 및 근거
- ORD 기록
- ord-4e3ac0425f334abfb729422afbe9f303
- 출처 데이터셋
- uspto-grants-1995_02
- 특허 번호
- US05389641
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