反应详情

温度

0 °C

Diisopropylethylamine (1.80 mL, 10.3 mmol) is added to a stirred suspension of 2-(2-chloro-5-methylpyrimidin-4-yl)-benzo[b]thiophene-4-carboxylic acid (3.00 g, 9.84 mmol) in anhydrous dichloromethane (100 mL) at 0° C. under nitrogen to form a solution, then followed by the successive addition of C,C-bis-(4-methoxyphenyl)-methylamine (2.51 g, 10.3 mmol) and powdered 1H-benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (4.56 g, 10.3 mmol). The resultant mixture is allowed to stir at 0° C. for 1 hour, then at room temperature for 3 hours. Diethyl ether (50 mL) is added in small portions to the mixture, the mixture is stirred for another 10 minutes before filtration. After vacuum drying at 35° C., the crude title compound (5.19 g) is obtained as a tan solid. It is used without further purification.

1. customto form a solution
2. waitat room temperature for 3 hours
3. stirringthe mixture is stirred for another 10 minutes before filtration
4. customAfter vacuum drying at 35° C.