反应详情

A solution of Example Z (1.0 g, 0.0038 mol) and lithium hydroxide (0.950 g) in MeOH (10 mL) was stirred at RT for overnight. The mixture was acidified by 2N HCl to pH=5-6 and extracted by CH2Cl2 (3×50 mL). The combined organic layers were washed with H2O, dried (MgSO4) and concentrated in vacuo to yield 4-((1-methyl-3,5-dioxo-1,2,4-triazolidin-4-yl)methyl)benzoic acid (0.6 g, 64%). 1H NMR (CDCl3): 7.71 (d, J=8.4 Hz, 2H), 7.17 (d, J=8.4 Hz, 2H), 4.68 (s, 2H), 2.90 (s, 3H), 2.6 (s, 3H); MS (ESI) m/e: 249 (M+1).

1. extractionextracted by CH2Cl2 (3×50 mL)
2. washThe combined organic layers were washed with H2O
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo