تفاعل #1519077
ord-194b42d44d0a4f2688a95a18b501f24e
معادلة التفاعل
malonodinitrile
acetic anhydride
2,6-diethyl-3,5-dipropyl-pyran-4-one
→
2-(2,6-diethyl-3,5-dimethylpyran-4-ylidene)malononitrile
المردود 47.0%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1استخلاصwas extracted twice with ether (50 ml)
- 2غسيلThe combined organic phases were washed with water (2×50 ml) and with saturated NaCl-solution (1×30 ml)
- 3تجفيفAfter drying (Na2SO4)
- 4أخرىthe solvent was evaporated (HV)
- 5أخرىthe crude product was purified via FC (n-hexane/EtOAC 7:3)
الإجراء التجريبي
To a solution of 0.33 g (5 mmol) of malonodinitrile in 2.4 ml (25 mmol) acetic anhydride 1.20 g (5 mmol) of 2,6-diethyl-3,5-dipropyl-pyran-4-one (prepared according to J. Chem. Soc (C), 1967, 828-830) was added. After addition of 150 ml of water the resulting solution was extracted twice with ether (50 ml). The combined organic phases were washed with water (2×50 ml) and with saturated NaCl-solution (1×30 ml). After drying (Na2SO4), the solvent was evaporated (HV) and the crude product was purified via FC (n-hexane/EtOAC 7:3) yielding 0.54 g (47%) of 2-(2,6-diethyl-3,5-dimethylpyran-4-ylidene)malononitrile as a brown solid.