反应详情

温度

211 °C

Heat in a 211° C. oil bath, a stirring solution of (S)-2-(4-methoxybutyl)-piperazine 0.086 g, 0.49 mmol), and 2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulen-10-ylamine (0.114 g, 0.49 mmol) in NMP (1 mL) for 4 h. Cool to room temperature, dilute the solution with brine (15 mL) and extract with EtOAc (3×30 mL). Concentrate the organic layers under reduced pressure to a volume of 20 mL and wash with 75% brine (4×20 mL). Dry the organic layer over Na2SO4, and filter. Concentrate the mixture under reduced pressure and purify by silica gel chromatography eluting with 10% (33% 2 M NH3 in MeOH/64% EtOH)/CH2Cl2. Combine the purified fractions, concentrate under reduced pressure, azeotrope with CH2Cl2/hexanes and place under vacuum to give the title compound: brown solid (0.036 g), mass spectrum (m/e):385.08 (M+H).

1. temperatureCool to room temperature
2. extractionextract with EtOAc (3×30 mL)
3. concentrationConcentrate the organic layers under reduced pressure to a volume of 20 mL
4. washwash with 75% brine (4×20 mL)
5. dry with materialDry the organic layer over Na2SO4
6. filtrationfilter
7. concentrationConcentrate the mixture under reduced pressure
8. custompurify by silica gel chromatography
9. washeluting with 10% (33% 2 M NH3 in MeOH/64% EtOH)/CH2Cl2
10. concentrationconcentrate under reduced pressure, azeotrope with CH2Cl2/hexanes and place under vacuum