反应详情

Ethyl 4-methyl-3-nitrobenzoate (105 g) was dissolved in glacial acetic acid (4 1), followed by stirring. To the solution, a solution of sodium nitrite (32 g) in water (80 ml) was added at once at a temperature of 10° C. to 15° C., and the resultant mixture was stirred at room temperature for 3 days. After completion of the reaction, the reaction mixture was evaporated under reduced pressure to remove acetic acid. Water was added to the residue, and the precipitated crystals were collected by filtration. The collected crystals were washed with water and dried. The obtained crystals was further washed with methanol and diethyl ether, and dried to give ethyl indazol-6-yl carboxylate (90 g), m.p. 125°-126° C.

1. customAfter completion of the reaction
2. customthe reaction mixture was evaporated under reduced pressure
3. customto remove acetic acid
4. additionWater was added to the residue
5. filtrationthe precipitated crystals were collected by filtration
6. washThe collected crystals were washed with water
7. customdried
8. washThe obtained crystals was further washed with methanol and diethyl ether
9. customdried