反应详情

温度

105 °C

38.1 mg (0.5679 mmol) potassium cyanide and 239 μl (1.704 mmol) triethylamine (dry; Fluka) in 6 ml dry DMF, 182 μl trimethylchlorosilane (Fluka) are added within 10 min to a solution of 100 mg (0.30 mmol) of 8-chloro-1-(2-chloro-phenyl)-1H-imidazo[4,5-c]quinoline 5-oxide (Example 71). The reaction mixture is stirred for 48 h at ca. 100-110° C. bath temperature. The cold solution is filtered, the solvent is evaporated. The residue is purified by chromatography on silica gel (CH2Cl2-methanol 9:1). The compound can be crystallized from CH2Cl2-hexane. mp: 248-250° C.; MS: 339 (M++1); HPLC: tret=13.19 min (Grad 1).

1. filtrationThe cold solution is filtered
2. customthe solvent is evaporated
3. customThe residue is purified by chromatography on silica gel (CH2Cl2-methanol 9:1)
4. customThe compound can be crystallized from CH2Cl2-hexane
5. customtret=13.19 min (Grad 1)