反应详情

温度

60 °C

To a 150 mL round-bottomed flask equipped with magnetic stirring was added methyl 2-[4-benzylpiperazinyl]benzoate (Preparation XIII) (2.3 g, 7.4 mmol) in THF (60 mL). A soln of LiOH (Aldrich) (940 mg, 22 mmol) in H2O (20 mL), was added and the reaction mixture was heated at 60° C. for 12 h. After cooling to RT, the reaction mixture was concentrated in vacuo and diluted with EtOAc (100 mL). A 10% soln of citric acid (25 mL) was added, the organic layer was separated and the aqueous layer was extracted with EtOAc (2×25 mL). The organic layers were combined, washed with H2O, satd NaCl, dried over Na2SO4, filtered and concentrated in vacuo to afford 2-[4-benzylpiperazinyl]benzoic acid as a white solid (2.05 g). MS (ESI, pos. ion) m/z: 297 (M+H). Calc'd for C18H20N2O2: 296.15: 296.15.

1. customTo a 150 mL round-bottomed flask equipped
2. temperatureAfter cooling to RT
3. concentrationthe reaction mixture was concentrated in vacuo
4. additiondiluted with EtOAc (100 mL)
5. additionA 10% soln of citric acid (25 mL) was added
6. customthe organic layer was separated
7. extractionthe aqueous layer was extracted with EtOAc (2×25 mL)
8. washwashed with H2O
9. dry with materialdried over Na2SO4
10. filtrationfiltered
11. concentrationconcentrated in vacuo