HRID2278842
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
1.000 g (purity 67%, approx. 2.357 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine-3-carboximidohydrazide in 15 ml of absolute ethanol were initially introduced and admixed with 1.557 g (7.070 mmol) of diethyl 2-fluoro-2-methyl-3-oxobutanedioate (described in J. Med. Chem. 1966, 9, 149-151). The mixture was stirred at RT overnight and then concentrated. The residue was purified by preparative HPLC (mobile phase: methanol/water, gradient 30:70→95:5). This gave 230 mg of the target compound (purity 95%; 21% of theory).
WORKUP
后处理
- concentrationconcentrated
- customThe residue was purified by preparative HPLC (mobile phase: methanol/water, gradient 30:70→95:5)