3-甲基噻唑烷-2,4-二酮

反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: At 0° C., N,N-dimethylformamide (2 mL, 27 mmol) was added to a solution of 3-methyl-thiazolidine-2,4-dione (33a) (1.77 g, 13.5 mmol) in phosphorus oxychloride (3.77 mL, 40.5 mmol). The reaction mixture was stirred at 110° C. for 3 hours, cooled to room temperature and quenched with a mixture of ice and ethyl acetate. The organic layer was washed with water (30 mL), brine (30 mL), dried over sodium sulfate, filtered, and evaporated under reduced pressure to give the desired aldehyde (33b) as a yellow solid (1.9 g, 10.7 mmol, 79%). cooled to room temperature quenched with a mixture of ice and ethyl acetate The organic layer was washed with water (30 mL), brine (30 mL) dried over sodium sulfate filtered evaporated under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of toluene (80 mL), piperidine (380 μL), acetic acid (380 μL), 3-(1,4,4,6-Tetramethyl-2-oxo-1,2,3,4-tetrahydro-quinolin-7-yl)-4-trifluoromethoxy-benzaldehyde (7.5 g, 19.16 mmol) and a 3-alkyl—thiazolidine-2,4-dione such as 3-Methyl-thiazolidine-2,4-dione (19.16 mmol) is heated at reflux overnight. The reaction mixture is cooled to room temperature, diluted with ethyl acetate and is washed with water and brine, dried over MgSO4. The residue is recrystallized to afford 3-methyl-5-[3-(1,4,4,6-tetramethyl-2-oxo-1,2,3,4-tetrahydro-quinolin-7-yl)-4-trifluoromethoxy-benzylidene]-thiazolidine-2,4-dione. at reflux overnight is washed with water and brine dried over MgSO4 The residue is recrystallized

反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: At 0° C., N,N-dimethylformamide (2 mL, 27 mmol) was added to a solution of 3-methyl-thiazolidine-2,4-dione (33a) (1.77 g, 13.5 mmol) in phosphorus oxychloride (3.77 mL, 40.5 mmol). The reaction mixture was stirred at 110° C. for 3 hours, cooled to room temperature and quenched with a mixture of ice and ethyl acetate. The organic layer was washed with water (30 mL), brine (30 mL), dried over sodium sulfate, filtered, and evaporated under reduced pressure to give the desired aldehyde (33b) as a yellow solid (1.9 g, 10.7 mmol, 79%). cooled to room temperature quenched with a mixture of ice and ethyl acetate The organic layer was washed with water (30 mL), brine (30 mL) dried over sodium sulfate filtered evaporated under reduced pressure