تفاعل #80291

معادلة التفاعل

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

hydrochloric acid

tin

→

desired product

المردود 79.3%

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

المردود 79.3%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe solid was filtered off
2. 2
   تركيزresidue was concentrated under reduced pressure
3. 3
   استخلاصextracted with ethyl acetate
4. 4
   غسيلThe organic layer was washed with water
5. 5
   تجفيفdried over anhydrous sodium sulfate
6. 6
   أخرىThe residue obtained by concentration under reduced pressure
7. 7
   أخرىwas crystallized from isopropyl ether

الإجراء التجريبي

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.

المصدر