반응 #59892

반응 방정식

2,3,5-trimethyl-4-nitropyridine1-oxide

acetyl chloride

→

title compound

4-chloro-2,3,5-trimethylpyridine 1-oxide

반응 조건

후처리

1. 1
   농축After the reaction mixture was concentrated
2. 2
   세척the residue was subjected to silica gel column chromatography (NH silica gel: 300 g, elution solvent: heptane, heptane/ethyl acetate=50/50, ethyl acetate, ethyl acetate/methanol=10/1)
3. 3
   기타to obtain fractions

실험 절차

The 2,3,5-trimethyl-4-nitropyridine1-oxide (13.4 g, 73.6 mmol) obtained in the step (11c) was added to acetyl chloride (80 ml, 1,125 mmol) at −30° C. in a nitrogen atmosphere. The mixture was stirred at −30° C. to room temperature for 4 hours and 20 minutes. After the reaction mixture was concentrated, the residue was subjected to silica gel column chromatography (NH silica gel: 300 g, elution solvent: heptane, heptane/ethyl acetate=50/50, ethyl acetate, ethyl acetate/methanol=10/1) to obtain fractions containing a pure product of the title compound and fractions containing a crude product of the title compound.

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