反应详情

温度

80 °C

Under an atmosphere of nitrogen to a suspension of 14.85 g of 5-chlorothiophen-2-carboxylic acid-{(R)-2-hydroxy-3-[4-(3-oxomorpholin-4-yl)phenylamino]propyl}amide (MW=409.89; 1 eq.) in 145 mL toluene and 22 mL N-methylpyrrolidone were added 7.13 g (MW=162.15; 1.2 eq.) of 1,1′-carbonyldiimidazol. The reaction mixture was heated to 80° C. After stirring for 30 minutes the mixture was heated to 110° C. and stirred at this temperature for 2 hours. Then the mixture was cooled to 22° C. After stirring for 1 hour at ambient temperature the product was isolated by filtration and washed with 60 mL of toluene and 60 mL of water. The wet product was dried at 30° C. in vacuo to yield 15.99 g (MW=435.89; 1.013 eq.) of the title compound (90% of theory).

1. temperaturewas heated to 110° C.
2. stirringstirred at this temperature for 2 hours
3. temperatureThen the mixture was cooled to 22° C
4. stirringAfter stirring for 1 hour at ambient temperature the product
5. customwas isolated by filtration
6. washwashed with 60 mL of toluene and 60 mL of water
7. customThe wet product was dried at 30° C. in vacuo