反応 #80272

反応方程式

5-(4,6-dimethoxypyrimidin-2-yl)oxy-4-formyl-3-methylbenzothiophene

potassium permanganate

→

desired compound

収率 76.0%

5-(4,6-dimethoxypyrimidin-2-yl)oxy-3-methylbenzothiophene -4-carboxylic acid

収率 76.0%

溶媒

acetone

water

反応条件

後処理

1. 1
   workup.ADDITIONwas dropwise added
2. 2
   workup.STIRRINGthe mixture was further stirred at room temperature for 4 hours
3. 3
   濃縮It was then concentrated under reduced pressure
4. 4
   その他to remove acetone
5. 5
   workup.ADDITIONa saturated sodium bicarbonate aqueous solution was added
6. 6
   抽出The mixture was extracted with ethyl acetate
7. 7
   その他the aqueous layer was precipitated with 10% hydrochloric acid
8. 8
   ろ過The precipitated crystals were collected by filtration
9. 9
   洗浄washed with water

実験手順

0.6 g of 5-(4,6-dimethoxypyrimidin-2-yl)oxy-4-formyl-3-methylbenzothiophene was dissolved in 80 ml of acetone. While stirring the solution at room temperature, 0.6 g of potassium permanganate dissolved in 10 ml of water was dropwise added thereto over a period of 15 minutes, and the mixture was further stirred at room temperature for 4 hours. It was then concentrated under reduced pressure to remove acetone, and then a saturated sodium bicarbonate aqueous solution was added thereto to make the mixture alkaline. The mixture was extracted with ethyl acetate, and then the aqueous layer was precipitated with 10% hydrochloric acid. The precipitated crystals were collected by filtration and washed with water to obtain 0.47 g (yield: 76%) of the desired compound.

出典