反应详情

To 1-(methoxycarbonyl)cyclopentanecarboxylic acid (630 mg, 3.7 mmol) in CH2Cl2/DMF (5:1, 37 mL) at 0° C. was added HOBT (730 mg, 4.8 mmol) and EDC (920 mg, 4.8 mmol). The mixture was stirred for 10 min then 3-methylbutylamine (640 mg, 7.4 mmol) was added and stirring was continued for 1 h. The solution was poured into water and the layers separated. The aqueous layer was extracted with methylene chloride and the combined extracts were washed with water, 1N HCl, sat'd NaHCO3, dried over magnesium sulfate, and concentrated to a glassy solid (800 mg, 90%). MS [M+H]+ 243.

1. stirringstirring
2. waitwas continued for 1 h
3. customthe layers separated
4. extractionThe aqueous layer was extracted with methylene chloride
5. washthe combined extracts were washed with water, 1N HCl
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated to a glassy solid (800 mg, 90%)