反应详情

Combine 2-chloro-3-(3,4-dichloro-phenyl)-pyrazine (0.124 g, 0.477 mmol) and piperazine (1.40 gm; 16.3 mmol) and heat the mixture for 2 hr. at 120° C. Cool to room temperature, and add DCM (50 mL) and water (50 mL). Separate the layers and extract the aqueous layer with DCM (2×25 mL). Combine the organic layers, wash with brine, dry (MgSO4) and concentrate. Purify via chromatography on silica gel eluting 0-15% methanol in DCM to give the title preparation (0.118 gm, 80%). MS (ES+) m/z: 310 (M+H)+.

1. customat 120° C
2. customSeparate the layers
3. extractionextract the aqueous layer with DCM (2×25 mL)
4. washCombine the organic layers, wash with brine
5. dry with materialdry (MgSO4)
6. concentrationconcentrate
7. customPurify via chromatography on silica gel eluting 0-15% methanol in DCM
8. customto give the title
9. custompreparation (0.118 gm, 80%)