反应详情

温度

17.5 °C

A solution of CrO3 (26.5 g) in a mixture of 15 ml of H2O and 235 ml of AcOH was prepared by sonicating the suspension for 45 min. The resulting solution was added dropwise to a cooled solution of N-(6-nitro-indan-5-yl)-acetamide (22 g, 0.1 mol) in Ac20 (2.5 L) while maintaining the temperature between 15-20° C. After the addition was completed, the mixture was stirred at 25° C. overnight, poured into 10 L of water, and stirred for 1 h. The solution was then extracted with two 2-L portions of CH2Cl2. The organic layers were combined, and concentrated to 500 ml, washed with two 50-ml portions of 10% NaOH followed by water, and then dried (Na2SO4). The solvent was removed, leaving a yellow powder (16 g, 75%), which was used for next step without further purification.

1. customwas prepared
2. customby sonicating the suspension for 45 min
3. additionAfter the addition
4. stirringstirred for 1 h
5. extractionThe solution was then extracted with two 2-L portions of CH2Cl2
6. concentrationconcentrated to 500 ml
7. washwashed with two 50-ml portions of 10% NaOH
8. dry with materialdried (Na2SO4)
9. customThe solvent was removed