反应详情

Methyl 3,5-bis(2′-decyltetradecanamido)benzoate from Step 2, potassium hydroxide (0.38 g, 5.77 mmol), and methanol (20 mL) were added to a 50 mL vessel and heated to reflux. Deionized water (10 mL) was then added and the reaction was held at reflux overnight. The reaction was then cooled to room temperature, which resulted in the formation of an oil phase. Diethyl ether (20 mL) was added and the aqueous phase was removed. The organic phase was then washed successively with 1 Molar hydrochloric acid (30 mL), 0.1 Molar hydrochloric acid (30 mL), and deionized water twice (30 mL each), before concentrating the ether layer by rotary evaporation and drying in vacuo to give 3,5-bis(2′-decyltetradecanamido)benzoic acid as a light brown waxy solid (1.33 g, 99%). The product was identified by 1H and 13C NMR spectroscopy and ESI-MS and was of satisfactory purity. The product was believed to be of the formula

1. temperatureheated to reflux
2. temperatureat reflux overnight
3. customwhich resulted in the formation of an oil phase
4. customthe aqueous phase was removed
5. washThe organic phase was then washed successively with 1 Molar hydrochloric acid (30 mL), 0.1 Molar hydrochloric acid (30 mL)
6. concentrationbefore concentrating the ether layer
7. customby rotary evaporation
8. customdrying in vacuo