反应详情

温度

0 °C

A solution of 9-fluorene carboxylic acid (2.10 g, 10.0 mmol) in 50 mL of CH2Cl2 was treated with oxalyl chloride in dichloromethane (6.0 mL, 12.0 mmol) and two drops of DMF. After 0.75 h, the mixture was concentrated under reduced pressure to give a white solid. The solid was diluted with 50 mL of CH2Cl2, cooled to 0° C., treated with ethylamine (1.0 g, 22 mmol). The transparent yellow solution was stirred for 3 h at room temperature and diluted with ethyl acetate and water. The organic fraction was dried over Na2SO4 and concentrated to a white solid. The solid purified by trituration with hexanes and recrystalization from hot methanol to give 2.60 g (86%) of title compound as white flakes. mp 233°-234° C.

1. concentrationthe mixture was concentrated under reduced pressure
2. customto give a white solid
3. dry with materialThe organic fraction was dried over Na2SO4
4. concentrationconcentrated to a white solid
5. customThe solid purified by trituration with hexanes and recrystalization from hot methanol