反应详情

温度

40 °C

To crude methyl 4-cyclobutyl-2-methyl-5-(4H-1,2,4-triazol-3-yl)benzoate (compound 202.2, 0.24 mmol, 1.0 equiv) from the previous step in a 4-mL vial was added methanol (1.5 mL) and water (0.5 mL) and lithium hydroxide monohydrate (20 mg, 0.48 mmol, 2.0 equiv), The resulting mixture was stirred at 40° C. for 42 hours. The reaction mixture was diluted into water (5 mL), acidified to pH 3 with 1M H3PO4 and extracted with DCM (3×5 mL). The organics were dried (Na2SO4), filtered and concentrated in vacuo to obtain the title compound as a white solid (61 mg, 98% over 2 steps). m/z (ES+) 258 (M+H)+.

1. extractionextracted with DCM (3×5 mL)
2. dry with materialThe organics were dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo