تفاعل #2073544
ord-525188c6465448da8fdc69741a6f1dbf
معادلة التفاعل
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1استخلاصextracted with ethyl acetate
- 2تجفيفThe separated organic layer was dried over MgSO4
- 3ترشيحfiltered
- 4تركيزconcentrated
- 5أخرىto give a dark oil
- 6درجة الحرارةthe solution was heated at 100° C. for 4 hours
- 7درجة الحرارةthen cooled
- 8تركيزconcentrated in-vacuo
الإجراء التجريبي
The product from Step 3 (2.54 g crude) and cyanoacetic acid (0.88 g, 10.4 mmol) were dissolved in DMF (10 mL) and Et3N (3.6 mL) was added. To the solution was added EDC (2.2 g, 11.4 mmol), and the mixture was allowed to stir at rt for 2 days. The reactin mixture was poured into water and extracted with ethyl acetate. The separated organic layer was dried over MgSO4, filtered, and concentrated to give a dark oil. The oil was dissolved in AcOH (5 mL) and the solution was heated at 100° C. for 4 hours then cooled and concentrated in-vacuo to give the title compound as a dark foam that was taken on without further purification. MS (ES+) m/e 540 [M+H]+.