反応 #5001

反応方程式

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

hydroxyamine hydrochloride

potassium acetate

→

aimed compound

収率 72.0%

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

収率 72.0%

溶媒

methanol

反応条件

後処理

1. 1
   workup.DISTILLATIONMethanol was distilled off under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   洗浄The organic layer was washed with water, 5% hydrochloric acid
4. 4
   乾燥a saturated salt aqueous solution, and was dried with magnesium sulfate anhydride
5. 5
   ろ過After 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
   ろ過The Florisil was filtered out
9. 9
   workup.DISTILLATIONethyl acetate was distilled off under reduced pressure

実験手順

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%.

出典