反应详情

To a solution of Example 5 (500 mg, 2.84 mmol) in dichloromethane (10 mL) was added 1,3-diisopropylcarbodiimide (0.44 mL, 2.84 mmol), 1-hydroxybenzotriazole hydrate (115 mg, 0.85 mmol), and di-t-butyl iminodiacetate (1.04 g, 4.26 mmol). The mixture was stirred at room temperature for about 24 hours, quenched with water, and extracted with diethyl ether. The combined organic extracts were washed with brine and saturated aqueous sodium bicarbonate, dried (Na2SO4), filtered and concentrated under vacuum. The residue was purified by flash column chromatography on silica gel using hexane/ethyl acetate (1:1) as the mobile phase to provide the desired product. MS (ESI): m/z 402 (M−H)−.

1. customquenched with water
2. extractionextracted with diethyl ether
3. washThe combined organic extracts were washed with brine and saturated aqueous sodium bicarbonate
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residue was purified by flash column chromatography on silica gel