反应详情

温度

60 °C

(3aRS,7aRS)-7,7-bis-(3-fluorophenyl)-2-vinyloxycarbonyl-4-perhydroisoindolone (64.5 g) is treated with a 6N solution (330 cc) of hydrochloric acid in dioxane for 30 minutes at 25° C. The solution is concentrated to dryness under reduced pressure (2.7 kPa) and the residue is taken up in ethanol (500 cc). The solution is heated at 60° C. for 6 hours and stirred for 16 hours at 25° C. and then concentrated to half its volume under reduced pressure (2.7 kPa) and the crystals formed are drained and washed with isopropyl ether and then dried. 7,7-Bis(3-Fluorophenyl)-4-perhydroisoindolone hydrochloride (48.7 g) is obtained. m.p.=264° C.

1. concentrationThe solution is concentrated to dryness under reduced pressure (2.7 kPa)
2. concentrationconcentrated to half its volume under reduced pressure (2.7 kPa)
3. customthe crystals formed
4. washwashed with isopropyl ether
5. customdried