反应详情

温度

115 °C

A mixture of 2-(3-{3-[4-acetyl-5-benzyloxy-2-ethylphenoxy]propoxy}-2-propylphenoxy)benzoic acid methyl ester (3.07 g, 5.04 mmol) and dimethylformamide dimethylacetal (0.9 mL, 7 mmol) in N,N-dimethylformamide (3 mL) was heated at 110-120° C. for 35 h. The mixture was cooled to room temperature and diluted with a mixture of ethyl acetate and 1 N hydrochloric acid. The organic layer was separated, washed twice with water, once with saturated sodium chloride solution, dried (sodium sulfate), filtered, and concentrated in vacuo. Chromatography (silica gel, 30% ethyl acetate/70% hexane to ethyl acetate) of the residue provided 2.1 g (63%) of the title compound as a yellow oil. TQF MS ES+ exact mass calculated for C40H46NO7 (p+1): m/z=652.3274. Found: 652.3270. IR (CHCl3, cm−1) 2965, 1720, 1605. Anal. Calcd for C40H45NO7: C, 73.71; H, 6.96; N, 2.15. Found: C, 73.72; H, 6.95; N, 2.18.

1. temperatureThe mixture was cooled to room temperature
2. customThe organic layer was separated
3. washwashed twice with water, once with saturated sodium chloride solution
4. dry with materialdried (sodium sulfate)
5. filtrationfiltered
6. concentrationconcentrated in vacuo