반응 #5001

반응 방정식

methyl 2-[(4,6-dimethoxypyrimidin-2-yl)oxy]-6-formylbenzoate

hydroxyamine hydrochloride

potassium acetate

→

aimed compound

수율 72.0%

methyl 2-[[4,6-dimethoxypyrimidin-2-yl)oxy]-6-(hydroxyiminomethyl)benzoate

수율 72.0%

용매

methanol

반응 조건

후처리

1. 1
   workup.DISTILLATIONMethanol was distilled off under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   세척The organic layer was washed with water, 5% hydrochloric acid
4. 4
   건조a saturated salt aqueous solution, and was dried with magnesium sulfate anhydride
5. 5
   여과After filtering
6. 6
   workup.ADDITIONa small amount of Florisil was added to the resultant product
7. 7
   workup.STIRRINGwas stirred for 5 minutes
8. 8
   여과The Florisil was filtered out
9. 9
   workup.DISTILLATIONethyl acetate was distilled off under reduced pressure

실험 절차

2.0 g of methyl 2-[(4,6-dimethoxypyrimidin-2-yl)oxy]-6-formylbenzoate, 0.8 g of hydroxyamine hydrochloride, 1.1 g of potassium acetate and 10 ml of methanol were placed in a 50 ml eggplant type flask, and were stirred for 10 minutes at room temperature. Methanol was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The organic layer was washed with water, 5% hydrochloric acid and a saturated salt aqueous solution, and was dried with magnesium sulfate anhydride. After filtering, a small amount of Florisil was added to the resultant product, and was stirred for 5 minutes. The Florisil was filtered out, and ethyl acetate was distilled off under reduced pressure to obtain 1.5 g of the aimed compound (refractive index=1.5558) at a yield of 72%.

출처