تفاعل #411779
ord-27b91a525a8f4762a5363865f4505b8c
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1workup.WAITthe mixture is left
- 2ترشيحAfter filtering
- 3أخرىthe filtrate is partitioned between water and dichloromethane
- 4أخرىThe phases are separated
- 5غسيلthe organic phase is washed successively with water, twice with an 0.2N solution of NaOH and water
- 6تجفيفdried over sodium sulfate
- 7ترشيحAfter filtering
- 8أخرىthe solvent is removed in vacuo
- 9أخرىthe 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.