반응 #7155

반응 방정식

7-Nitro-1-tetralone

pyridine-2-aldehyde

piperidine

acetic acid

→

7-nitro-1-oxo-2-(2-pyridylmethylidene)-1,2,3,4-tetrahydronaphthalene

수율 19.1%

용매

toluene

반응 조건

후처리

1. 1
   온도the mixture is heated
2. 2
   온도under reflux for 12 hours
3. 3
   세척The reaction solution is washed with water
4. 4
   건조the organic layer is dried over sodium sulfate
5. 5
   기타The solvent is evaporated under reduced pressure
6. 6
   기타The residue is purified by silica gel chromatography (eluent: gradient from 0% to 100% hexane/ethyl acetate)

실험 절차

7-Nitro-1-tetralone (500 mg), pyridine-2-aldehyde (315 mg), piperidine (0.15 ml) and acetic acid (0.4 ml) are dissolved in toluene (10 ml), and the mixture is heated under reflux for 12 hours. The reaction solution is washed with water, and the organic layer is dried over sodium sulfate. The solvent is evaporated under reduced pressure. The residue is purified by silica gel chromatography (eluent: gradient from 0% to 100% hexane/ethyl acetate) to give 7-nitro-1-oxo-2-(2-pyridylmethylidene)-1,2,3,4-tetrahydronaphthalene (140 mg).

출처