تفاعل #40709

معادلة التفاعل

4-acetylbenzaldehyde

morpholine

→

yellowish oil

1-[4-(Morpholin-4-ylmethyl)phenyl]ethanone

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةto reflux for 3 hours
3. 3
   تركيزThe mixture was concentrated
4. 4
   workup.ADDITIONThe residue was mixed with ethyl acetate
5. 5
   غسيلwashed with sat. NaHCO3 solution and sat. NaCl solution
6. 6
   أخرىDrying
7. 7
   أخرىevaporation of the mixture
8. 8
   أخرىresulted in a crude product which
9. 9
   أخرىwas purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 40-80%)

الإجراء التجريبي

4.7 g of 1,4-dihydro-2,6-dimethyl-3,5-pyridinecarboxylate and 1.3 g of scandium triflate were added to 2.75 g of 4-acetylbenzaldehyde (18.56 mmol), 1.7 ml of morpholine and 3 g of 4 Å molecular sieves in 100 ml of tetrahydrofuran under argon, and the mixture was heated to reflux for 3 hours. The mixture was concentrated. The residue was mixed with ethyl acetate and washed with sat. NaHCO3 solution and sat. NaCl solution. Drying and evaporation of the mixture resulted in a crude product which was purified by chromatography on silica gel (eluent: cyclohexane/ethyl acetate 40-80%). 1.85 g of a yellowish oil were obtained.

المصدر