反应详情

To a solution of 2-chloro-5-iodobenzoic acid (1.0 g, 3.54 mmol) in 40 mL DMF was added diisopropylethyl amine (1.23 mL, 7.08 mmol) followed by HATU (2.02 g, 5.31 mmol). After stirring the reaction at room temperature for 10 min, N-hydroxy-2,2-dimethylpropanimidamide (0.82 g, 7.08 mmol) was added. The resulting reaction mixture was stirred at room temperature for 1 h and then at 110° C. for 16 h. After cooling to room temperature the reaction was quenched with water and extracted with ethyl acetate. The combined organic fractions were washed with brine, dried (Na2SO4), concentrated, and purified by flash chromatography (2-5% EtOAc in hexanes) to yield 660 mg of intermediate US1-2.

1. customthe reaction at room temperature for 10 min
2. customThe resulting reaction mixture
3. stirringwas stirred at room temperature for 1 h
4. customwas quenched with water
5. extractionextracted with ethyl acetate
6. washThe combined organic fractions were washed with brine
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated
9. custompurified by flash chromatography (2-5% EtOAc in hexanes)