反应详情

A mixture of 6-bromo-2-(4-cyclopropylpiperazin-1-yl)benzothiazole (480 mg, 1.42 mmol), acetamide (251 mg, 4.26 mmol), Pd(OAc)2 (15.9 mg, 0.071 mmol), Cs2CO3 (694 mg, 2.13 mmol) and xantphos (62 mg, 0.107 mmol) in 1,4-dioxane (10 mL) was heated at reflux for 12 h. Water (5 mL) was added and the mixture was filtered. The filtrate was extracted with EtOAc (3×5 mL). The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated to give a residue, which was purified by the preparative HPLC to give 108 mg (24%) of N-[2-(4-cyclopropylpiperazin-1-yl)benzothiazol-6-yl]acetamide as a trifluoroacetate salt.

1. temperaturewas heated
2. temperatureat reflux for 12 h
3. filtrationthe mixture was filtered
4. extractionThe filtrate was extracted with EtOAc (3×5 mL)
5. washThe combined organic extracts were washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customto give a residue, which
9. customwas purified by the preparative HPLC