反应详情

4-Cyclohexyl-benzoyl chloride (0.67 mmol) was added under nitrogen to a suspension of 5-bromo-6-(1-methoxycarbonyl-2-phenyl-ethoxy)-naphthalen-2-ylmethyl-ammonium; chloride (0.30 g, 0.67 mmol), prepared in step 3 of Example 53, in 20 mL of methylene chloride at room temperature. Triethylamine (0.186 mL, 1.33 mmol) was then added to the mixture. After the addition the reaction was stirred at room temperature for 18 h (overnight). The reaction was diluted with methylene chloride, extracted one time with 1N HCl and two times with 5% NaHCO3. The organic layer was separated, dried (MgSO4) and the solvent removed under reduced pressure to give 2-{1-bromo-6-[(4-cyclohexyl-benzoylamino)-methyl]-naphthalen-2-yloxyl}-3-phenyl-propionic acid methyl ester (0.3362 g, 84%) as an off-white solid, mp 160-161° C.

1. additionAfter the addition the reaction
2. extractionextracted one time with 1N HCl and two times with 5% NaHCO3
3. customThe organic layer was separated
4. dry with materialdried (MgSO4)
5. customthe solvent removed under reduced pressure