反应详情

温度

110 °C

Combine 9-fluoro-11H-12-thia-6,11-diaza-dibenzo[a,f]azulen-5-ylamine hydrogen chloride (510.2 mg, 1.6 mmol, (S)-2-(2-methoxy-ethyl) piperazine (460.8 mg, 3.2 mmol) and diisopropylethyl amine (206 mg, 1.6 mmol) in DMSO (0.75 mL) and toluene (3.0 mL), stir and heat to 110° C. After 55 hours, cool the reaction to RT, dilute with CH2Cl2, wash with H2O and Brine. Dry the organic layer with by Na2SO4. The crude material pass through a 5 g SCX column, collect the 0.2 N NH3/MeOH eluent, concentrate to a residue, which purified by chromatography on silica gel, gradient (100% CH2Cl2 to 100% CH2Cl2: 2N NH3/MeOH=15:1), give 410 mg of title compound. Mass spectrum: ACPI (m/e): 411.2 (M+1).

1. temperaturecool
2. customthe reaction to RT
3. washwash with H2O and Brine
4. dry with materialDry the organic layer with by Na2SO4
5. customThe crude material pass through a 5 g SCX column, collect the 0.2 N NH3/MeOH eluent
6. concentrationconcentrate to a residue, which
7. custompurified by chromatography on silica gel, gradient (100% CH2Cl2 to 100% CH2Cl2: 2N NH3/MeOH=15:1)