反应详情

温度

80 °C

Sulfuric acid (4.00 mL, 47.3 mmol) was added to a mixture of 1-benzhydryl-3-hydroxyazetidine-3-carboxylic acid (2.13 g, 7.50 mmol) in MeOH (20 mL). The mixture was heated to 80° C. for 18 h, diluted with EtOAc, extracted with water, 1N NaOH, dried over MgSO4, and evaporated. The solid was rinsed with Et2O to give methyl 1-benzhydryl-3-hydroxyazetidine-3-carboxylate. 1H NMR (300 MHz, CDCl3) δ ppm 7.43-7.49 (m, 4H), 7.24-7.31 (m, 4H), 7.15-7.23 (m, 2H), 4.54 (s, 1H), 3.90 (s, 3H), 3.59-3.72 (m, 2H), 3.24-3.39 (m, 2H). MS (ESI) m/z: Calculated; 297.14 Observed: 298.1 (M++1).

1. extractionextracted with water, 1N NaOH
2. dry with materialdried over MgSO4
3. customevaporated
4. washThe solid was rinsed with Et2O