反应详情

温度

50 °C

To a solution of methyl 2-{[(4-fluorophenyl)methyl]oxy}-4-(1-methyl-1H-pyrazol-4-yl)-5-(4-morpholinylmethyl)benzoate (may be prepared as described in Description 18; 155 mg, 0.353 mmol) in tetrahydrofuran (4 ml) was added lithium hydroxide (31 mg, 1.29 mmol) followed by water (1 ml). The mixture was heated at 50° C. for one hour. 2M hydrochloric acid (0.79 ml, 1.59 mmol) was added and the solvent removed in vacuo. The residue was redissolved in N,N-dimethylformamide (4 ml) and diisopropylethylamine (0.12 ml, 0.71 mmol), 3-aminopyridine (43.2 mg, 0.46 mmol), 1-hydroxy-7-azabenzotriazole (57.6 mg, 0.42 mmol) and EDC (101 mg, 0.53 mmol) were added. The solution was stirred overnight, then the solvent was removed in vacuo to give a residue. Purification by MDAP yielded the title compound as a white solid. 84 mg.

1. customthe solvent removed in vacuo
2. dissolutionThe residue was redissolved in N,N-dimethylformamide (4 ml)
3. customthe solvent was removed in vacuo
4. customto give a residue
5. customPurification by MDAP