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
A solution of 1-[(diethoxyphosphoryl)methyl]-7-trifluoromethyl[1,2,4]triazolo[4,3-a]quinoxalin-4(5H)-one (750 mg, 1.85 mmol) in 20 ml of ethanol and 20 ml of 10% sodium hydroxide was stirred at room temperature for 1 h. The solvent was removed under reduced pressure, and the residue was dissolved in water and applied to an ion-exchange column (Amberlite IR-120, H+ -form) prewashed with 4M hydrochloric acid followed by deionized water. Elution with deionized water gave an acidic eluate, which was concentrated in vacuo to give 448 mg (65%) of the title compound, m.p. 276°-280° C. (from water); 1H-NMR (DMSO-d6): δ 1.16 (t, 3H), 3.98 (quint, 2H), 4.08 (d, 2H), 7.64 (d, 1H), 7.68 (s, 1H), 8.42 (d, 1H), 12.28 (s, 1H), MS: m/e 377 (MH+).
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- dissolutionthe residue was dissolved in water
- washElution with deionized water
- customgave an acidic eluate, which
- concentrationwas concentrated in vacuo