反应详情

Methyl 2-bromobenzo[d]thiazole-6-carboxylate (0.52 g, 1.90 mmol), Boc-piperazine (0.44 g. 2.38 mmol) and potassium carbonate (0.53 g, 3.80 mmol) were suspended in acetonitrile (21 ml) and refluxed overnight. The resulting mixture was then cooled to room temperature, concentrated in vacuo to approximately 2 ml, diluted with water and extracted with ethyl acetate. The organic layer was dried (MgSO4) and concentrated in vacuo to yield a residue which was treated with trifluoroacetic acid/dichloromethane (6 ml, 1:1) for 1.5 hrs. The resulting mixture was concentrated in vacuo, the resulting residue was dissolved in dichloromethane and washed with saturated sodium bicarbonate to yield methyl 2-(piperazin-1-yl)benzo[d]thiazole-6-carboxylate.

1. temperaturerefluxed overnight
2. concentrationconcentrated in vacuo to approximately 2 ml
3. additiondiluted with water
4. extractionextracted with ethyl acetate
5. dry with materialThe organic layer was dried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto yield a residue which
8. concentrationThe resulting mixture was concentrated in vacuo
9. dissolutionthe resulting residue was dissolved in dichloromethane
10. washwashed with saturated sodium bicarbonate