反応 #80291

反応方程式

allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methyl-3-nitroindol-4-carboxylate

hydrochloric acid

tin

→

desired product

収率 79.3%

Allyl 3-Amino-5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methylindol-4-carboxylate

収率 79.3%

溶媒

methanol

反応条件

後処理

1. 1
   ろ過The solid was filtered off
2. 2
   濃縮residue was concentrated under reduced pressure
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄The organic layer was washed with water
5. 5
   乾燥dried over anhydrous sodium sulfate
6. 6
   その他The residue obtained by concentration under reduced pressure
7. 7
   その他was crystallized from isopropyl ether

実験手順

3.4 g of allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methyl-3-nitroindol-4-carboxylate was dissolved in 50 ml of methanol, and 5 ml of concentrated hydrochloric acid was added thereto. Then, 4.9 g of tin powder was gradually added at room temperature. Them, the mixture was stirred at room temperature for 12 hours. The solid was filtered off, and then residue was concentrated under reduced pressure and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. The residue obtained by concentration under reduced pressure, was crystallized from isopropyl ether to obtain 2.5 g (yield: 79%) of the desired product. mp: 132°-135° C.

出典