反应详情

Triethylamine (1.4 cc) is added to a suspension of 2-(2-pyridyl)acetic acid hydrochloride (1.73 g) in dry dichloromethane (30 cc). The solution is cooled to +5° C. and then treated with N,N'-carbonyldiimidazole (1.62 g). The mixture is stirred for 15 minutes at +5° C. and a solution of (3aRS,7aRS)-7,7-diphenyl-4-perhydroisoindolone hydrochloride (3.27 g) and triethylamine (2.8 cc) in dichloromethane (20 cc) is then added. The reaction mixture is stirred at 20° C. for 2 hours and then concentrated to dryness under reduced pressure (2.7 kPa). The residue is taken up in a mixture of ethyl acetate (100 cc) and water (75 cc). The organic phase is washed with water (50 cc), dried over magnesium sulphate and filtered and the filtrate is concentrated to dryness under reduced pressure (2.7 kPa). The residue is recrystallized from a mixture of acetonitrile (30 cc) and isopropyl ether (30 cc). (3aRS,7aRS)-7,7-diphenyl-2-[2-(2-pyridyl)acetyl]-4-perhydroisoindolone (1.6 g) is obtained in the form of white crystals melting at 195° C.

1. temperatureThe solution is cooled to +5° C.
2. stirringThe reaction mixture is stirred at 20° C. for 2 hours
3. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
4. additionThe residue is taken up in a mixture of ethyl acetate (100 cc) and water (75 cc)
5. washThe organic phase is washed with water (50 cc)
6. dry with materialdried over magnesium sulphate
7. filtrationfiltered
8. concentrationthe filtrate is concentrated to dryness under reduced pressure (2.7 kPa)
9. customThe residue is recrystallized from a mixture of acetonitrile (30 cc) and isopropyl ether (30 cc)