反应详情

温度

20 °C

2 g (11.5 mmoles) of gallic acid, 2.5 g (11.5 mmoles) of 4-nitrophenetylamine hydrochloride, 1.8 g (11.5 mmoles) of hydrated 1-hydroxybenzotriazole, 2.25 g (11.5 mmoles) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 3.3 ml (23 mmoles) of triethylamine are introduced into a 100 ml flask containing 30 ml of anhydrous DMF. The orange-coloured solution obtained is agitated at 20° C. for 20 hours and diluted in a mixture of dichloromethane (50 ml) and water (30 ml). After decanting, the organic phase is washed with a molar solution of hydrochloric acid (20 ml) and with water (3×20 ml) until neutrality is achieved. After drying the organic phase over magnesium sulphate, followed by filtration and concentration under vacuum, the residue is purified on a silica gel column (eluant: dichloromethane/methanol: 9/1). The expected product is obtained in the form of a colourless oil with a yield of 42% (1.57 g).

1. customThe orange-coloured solution obtained
2. customAfter decanting
3. washthe organic phase is washed with a molar solution of hydrochloric acid (20 ml) and with water (3×20 ml) until neutrality
4. dry with materialAfter drying the organic phase over magnesium sulphate
5. filtrationfollowed by filtration and concentration under vacuum
6. customthe residue is purified on a silica gel column (eluant: dichloromethane/methanol: 9/1)