تفاعل #42859

ord-bfec5973ad2643fa973dabb9e9e42e5e

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
160°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was cooled to near room temperature
  2. 2
    استخلاصThe mixture was extracted with ethyl acetate three times
  3. 3
    غسيلThe organic layers were washed with a saturated sodium chloride aqueous solution
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated

الإجراء التجريبي

The mixture of 10 g of 3,3-dimethylsuccinic acid and 102.7 g of urea was stirred for 10 hours at 160° C. Into the reaction mixture was added water at 100° C., and the mixture was cooled to near room temperature. The mixture was extracted with ethyl acetate three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 7.8 g of 3,3-dimethylpyrrolidin-2,5-dione.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07732448B2uspto-grants-2010_06