反应详情

温度

100 °C

35.0 g (216 mmol) N,N-carbonyldiimidazole were added to 23.9 g (70.3 mmol) [2-(2-amino-5-methoxyphenyl)-ethyl]-(1-benzylpiperidin-4-yl)-amine in 175 mL DMF and the mixture was stirred for 2 h at 100° C. The reaction mixture was poured onto approx. 1 kg of ice water and stirred overnight. The precipitated product was suction filtered, washed with 100 mL water and dried at 45° C. in the CAD. The residue was stirred with 150 mL DIPE and suction filtered. The solid product was washed with 50 mL DIPE. After drying in the CAD at 35° C., 21.6 g of the desired product were obtained.

1. stirringstirred overnight
2. filtrationfiltered
3. washwashed with 100 mL water
4. customdried at 45° C. in the CAD
5. stirringThe residue was stirred with 150 mL DIPE and suction
6. filtrationfiltered
7. washThe solid product was washed with 50 mL DIPE
8. customAfter drying in the CAD at 35° C.