Potassium Cyanide → HCID 20092979、化合物
反応式
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]参加物
5
実験手順
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.
後処理
- 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.
出典と根拠
- ORDレコード
- ord-4e3ac0425f334abfb729422afbe9f303
- 出典データセット
- uspto-grants-1995_02
- 特許番号
- US05389641
反応ノート
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