反应详情

A mixture of 12.0 g. (0.04 mole) of 4-carbobenzoxypiperazine-2-carboxylic acid, 8.4 g. (0.06 mole) of o-nitrofluorobenzene, 16 g. of triethylamine and 100 ml. of dimethylsulfoxide is heated at 90° for 8 1/2 hours, cooled, diluted with water (300 ml.) and extracted with ether. The aqueous phase is then acidified with dilute hydrochloric acid and extracted with ether. The combined ether extracts are diluted with 1/3 its volume of pentane. The ether-pentane solution is washed with water, dried (MgSO4) and concentrated to give 14 g. of yellow-orange glassy product. Thin layer chromatrgraphy analysis (1% acetic acid in benzene on a silica gel plate) shows 1 main spot with a faint second impurity spot.

1. additionA mixture of 12.0 g
2. temperaturecooled
3. extractionextracted with ether
4. extractionextracted with ether
5. additionThe combined ether extracts are diluted with 1/3 its volume of pentane
6. washThe ether-pentane solution is washed with water
7. dry with materialdried (MgSO4)
8. concentrationconcentrated
9. customto give 14 g