反应详情

Trifluoroacetic acid (3 cc) is added to a solution of 4,4-bis(3-fluorophenyl)cyclohexenone (90.3 g) and N-butoxymethyl-N-(trimethylsilylmethyl)benzylamine (123 cc) in dry dichloromethane (1000 cc). The reaction mixture is brought to reflux, then stirred for 2 hours while allowing the temperature to return to 25° C. and for a further 15 minutes after the addition of potassium carbonate (60 g). After filtration and concentration to dryness under reduced pressure (2.7 kPa), the crystallized residue is stirred vigorously with isopropyl ether, drained, washed and recrystallized in cyclohexane (300 cc). The crystals are drained, washed with cyclohexane (2×15 cc) and dried to give (3aRS,7aRS)-2-benzyl-7,7-bis(3-fluorophenyl)perhydro-4-isoindolone (92 g) in the form of white crystals. M.p. 124° C.

1. temperatureto reflux
2. waitto return to 25° C. and for a further 15 minutes
3. filtrationAfter filtration and concentration to dryness under reduced pressure (2.7 kPa)
4. stirringthe crystallized residue is stirred vigorously with isopropyl ether
5. washwashed
6. customrecrystallized in cyclohexane (300 cc)
7. washwashed with cyclohexane (2×15 cc)
8. customdried