反应详情

温度

80 °C

To a solution of 9 g (29.92 mmol) of 6-amino-5-chloro-1H-indazole-7-carboxylic acid methyl ester in 68 mL of acetic acid at 80° C., is added dropwise 2 mL (38.89 mmol) of bromine. The mixture is stirred over the night at 80° C. The solvents are evaporated and water is added to the residue. The product is precipitated at pH 5 by addition of 1N aqueous NaOH, filtrated, washed with a minimum of water and dried under high vacuum. 1 g (3.28 mmol, 11%) of pure product is obtained; LC/MS:305/306 (M+H)+.

1. customThe solvents are evaporated
2. additionwater is added to the residue
3. customThe product is precipitated at pH 5 by addition of 1N aqueous NaOH
4. filtrationfiltrated
5. washwashed with a minimum of water
6. customdried under high vacuum