Reaktion #80291

Reaktionsgleichung

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

hydrochloric acid

tin

→

desired product

Ausbeute 79.3%

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

Ausbeute 79.3%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe solid was filtered off
2. 2
   Einengenresidue was concentrated under reduced pressure
3. 3
   Extraktionextracted with ethyl acetate
4. 4
   WaschenThe organic layer was washed with water
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   SonstigeThe residue obtained by concentration under reduced pressure
7. 7
   Sonstigewas crystallized from isopropyl ether

Vorschrift

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.

Quelle