تفاعل #83704

ord-7e0c0a8a08d54cafae99d5a80f6fa36a

المذيبات

ظروف التفاعل

درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلthe reaction mixture is washed with 100 cm3 of water
  2. 2
    تجفيفdried over magnesium sulphate
  3. 3
    تركيزconcentrated to dryness under reduced pressure (2.7 kPa)
  4. 4
    أخرىThe residue obtained
  5. 5
    أخرىis recrystallized in ethyl ether
  6. 6
    أخرىdried under reduced pressure (2.7 kPa)

الإجراء التجريبي

To a solution of 2.8 g of (3aRS,7RS,7aSR)-7-hydroxy-7-(2-methoxyphenyl)-4-perhydroisoindolone and 1.3 cm3 of triethylamine in 60 cm3 of anhydrous dichloromethane are added 1.55 g of (2-methoxyphenyl)acetic acid, 0.03 g of hydroxybenzotriazole hydrate and 1.96 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride. After stirring for 20 hours at 20° C., the reaction mixture is washed with 100 cm3 of water, dried over magnesium sulphate and then concentrated to dryness under reduced pressure (2.7 kPa). The residue obtained is recrystallized in ethyl ether and the crystals are drained and then dried under reduced pressure (2.7 kPa). 3.1 g of (3aRS,7RS,7aSR)-7-hydroxy-7-(2-methoxyphenyl)-2-[(2-methoxyphenyl)acetyl]-4-perhydroisoindolone are obtained, in the form of a white solid melting at 184° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05624950uspto-grants-1997_04