反应详情

To a stirred solution of 3-[5-chloro-3-(4-methyl-1-piperazinyl)-2-oxo-1(2H)-pyrazinyl]-4-methyl-benzoic acid, methyl ester (Example 107b) in tetrahydrofuran (6 mL) under nitrogen was added cyclopropylamine (0.15 mL) followed by iso-propylmagnesium chloride (2M in tetrahydrofuran, 0.8 mL), portionwise. After 1 h, sat. aqueous NH4Cl was added and the mixture extracted into ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4), filtered and the solvent removed in vacuo. Purification by preparative HPLC (Gemini column, 0.1% ammonia:acetonitrile eluent) afforded the title compound (35 mg).

1. extractionthe mixture extracted into ethyl acetate
2. washThe combined organic extracts were washed with brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customthe solvent removed in vacuo
6. customPurification by preparative HPLC (Gemini column, 0.1% ammonia:acetonitrile eluent)