반응 #80291

반응 방정식

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

hydrochloric acid

tin

→

desired product

수율 79.3%

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

수율 79.3%

용매

methanol

반응 조건

후처리

1. 1
   여과The solid was filtered off
2. 2
   농축residue was concentrated under reduced pressure
3. 3
   추출extracted with ethyl acetate
4. 4
   세척The organic layer was washed with water
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   기타The residue obtained by concentration under reduced pressure
7. 7
   기타was crystallized from isopropyl ether

실험 절차

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.

출처