تفاعل #411779

ord-27b91a525a8f4762a5363865f4505b8c

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITthe mixture is left
  2. 2
    ترشيحAfter filtering
  3. 3
    أخرىthe filtrate is partitioned between water and dichloromethane
  4. 4
    أخرىThe phases are separated
  5. 5
    غسيلthe organic phase is washed successively with water, twice with an 0.2N solution of NaOH and water
  6. 6
    تجفيفdried over sodium sulfate
  7. 7
    ترشيحAfter filtering
  8. 8
    أخرىthe solvent is removed in vacuo
  9. 9
    أخرىthe residue is chromatographed through silica gel

الإجراء التجريبي

24.59 g (132.8 mmol) of potassium phthalimide are added to a solution of 14.3 ml (124.4 mmol) of 5-chloro-2-pentanone in 100 ml of DMF and the mixture is left to stir at room temperature for 3 h and at 60° C. for 30 h. After filtering, the filtrate is partitioned between water and dichloromethane. The phases are separated and the organic phase is washed successively with water, twice with an 0.2N solution of NaOH and water and then dried over sodium sulfate. After filtering, the solvent is removed in vacuo and the residue is chromatographed through silica gel using heptane/ethyl acetate=6/4. 9.8 g (34%) of (14.1) are obtained after concentrating the product fractions.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06218415B1uspto-grants-2001_04