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
The solution of 2-isobutyl-N,N-bis(4-methoxybenzyl)imidazo[1,2-a]quinoxalin-4-amine (16 mg, 0.033 mmol) in 1 mL of trifluoroacetic acid was stirred at 70° C. for 6 hours. The solvent was removed under reduced pressure. And then 10 mL of saturated aqueous sodium bicarbonate was added. The resulting mixture was extracted with 75 mL of ethyl acetate. The organic layer was separated and then washed with water (15 mL), brine (15 mL), dried over MgSO4, filtered and concentrated. The crude product was purified by preparative TLC sheet (ethyl acetate and hexanes) to give the titled compound (6.3 mg, 79%). MS: MH+=241. 1H NMR (300 MHz, CDCl3): δ 7.74 (s, 1H), 7.68 (m, 2H), 7.30-7.40 (m, 4H), 5.70 (brs, 2H), 2.67 (d, 2H), 2.08 (m, 1H), 1.00 (d, 6H).
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- additionAnd then 10 mL of saturated aqueous sodium bicarbonate was added
- extractionThe resulting mixture was extracted with 75 mL of ethyl acetate
- customThe organic layer was separated
- washwashed with water (15 mL), brine (15 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by preparative TLC sheet (ethyl acetate and hexanes)