反应详情

A solution of 8 (0.035 g, 0.091 mmol), N-acetyl-homopiperizine (0.025 g, 0.18 μmol), excess potassium carbonate in DMF was heated at 80° C. resulting in a color change after 5 minutes. LC/MS and TLC indicated conversion to tosyl protected product after 15 minutes. 1 ml of 6N NaOH and 1 ml of methanol were added to the reaction resulting in the immediate removal the tosyl group by LC/MS (M+1=337). The reaction was partitioned between EtOAc/H2O and extracted. The crude product was purified by preparative HPLC giving 9 (0.022 g) as a clear oil in 73% yield.

1. customresulting in a color change after 5 minutes
2. customafter 15 minutes
3. customresulting in the immediate removal the tosyl group by LC/MS (M+1=337)
4. customThe reaction was partitioned between EtOAc/H2O
5. extractionextracted
6. customThe crude product was purified by preparative HPLC