反应详情

温度

40 °C

Under a nitrogen atmosphere, a mixture of 1-{[3-amino-7-(benzyloxy)quinolin-4-yl]amino}-2-methylpropan-2-ol (45.0 g, 0.133 mol) and acetonitrile (180 mL) was heated to 40° C. Acetoxyacetyl chloride (21.8 g, 0.160 mol) was added to the resulting gray suspension over a period of 15 minutes while maintaining the temperature at 55±5° C. during the addition. Following the addition, a precipitate formed, and the reaction was heated at 55° C. for 15 minutes. The reaction mixture was then cooled to ˜0° C., and the product was isolated by filtration, washed sequentially with a small amount of acetonitrile and acetone, and dried under vacuum at 50° C. to provide 57.6 g of 2-({7-benzyloxy-4-[(2-hydroxy-2-methylpropyl)amino]quinolin-3-yl}amino)-2-oxoethyl acetate hydrochloride.

1. temperaturewhile maintaining the temperature at 55±5° C.
2. additionduring the addition
3. additionthe addition
4. customa precipitate formed
5. temperaturethe reaction was heated at 55° C. for 15 minutes
6. temperatureThe reaction mixture was then cooled to ˜0° C.
7. customthe product was isolated by filtration
8. washwashed sequentially with a small amount of acetonitrile and acetone
9. customdried under vacuum at 50° C.