반응 #72870

반응 방정식

water

ethyl 1,5,5-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate

sodium ethoxide

→

title compound

수율 79.1%

Ethyl 6-(hydroxymethylene)-1,5,5-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate

수율 79.1%

용매

ethyl formate

반응 조건

후처리

1. 1
   온도refluxed for 3 hours
2. 2
   세척The aqueous layer was washed with diethyl ether (40 mL)
3. 3
   기타to remove unreacted
4. 4
   추출extracted with ethyl acetate (50 mL×2)
5. 5
   기타The organic extracts were collected
6. 6
   기타dried on Na2SO4
7. 7
   기타evaporated to dryness

실험 절차

A solution of ethyl 1,5,5-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate (1.00 g, 4 mmol) in anhydrous ethyl formate (10 mL) was treated with sodium ethoxide (0.54 g, 8 mmol) and refluxed for 3 hours. The mixture was cooled to room temperature and poured into cold water (40 mL). The aqueous layer was washed with diethyl ether (40 mL) to remove unreacted starting material, acidified with a 20% NaH2PO4 solution and extracted with ethyl acetate (50 mL×2). The organic extracts were collected, dried on Na2SO4 and evaporated to dryness to obtain the title compound (0.88 g, 78.8% yield) as a brown solid.

출처