反应详情

温度

60 °C

To a suspension of 6-(2-fluoro-4-iodo-phenylamino)-1-oxo-2,3-dihydro-1H-isoindole-5-carboxylic acid methyl ester (220 mg, 0.52 mmol) in IMS (7 mL) was added aqueous sodium hydroxide solution (1.3 mL, 1M, 1.30 mmol). The reaction mixture was heated at 60° C. for 3 hours, during which the solids dissolved. The reaction mixture was concentrated in vacuo to remove the IMS and the resultant solution was acidified to pH ˜5 by addition of aqueous hydrochloric acid (1M) causing a precipitate to form. The product was collected by filtration and dried under vacuum at 45° C. to yield the title compound as a brown solid (250 mg, >100%). LCMS (Method B): RT=3.07 min, M+MeCN+H+=454.

1. dissolutiondissolved
2. concentrationThe reaction mixture was concentrated in vacuo
3. customto remove the IMS
4. additionthe resultant solution was acidified to pH ˜5 by addition of aqueous hydrochloric acid (1M)
5. customto form
6. filtrationThe product was collected by filtration
7. customdried under vacuum at 45° C.