反应详情

2.08 g (5.0 mmol) of 4-[3-(1-ethoxycarbonyl-1-methyl-ethoxy)-benzoylamino]-piperidine-1-carboxylic acid tert-butyl ester was dissolved under argon in 80 mL of MeCl2; to the stirred solution, 3.66 mL (5.46 g=10 eq.) of TFA was added drop by drop and stirring continued at rt for 5 h. Then, the reaction mixture was evaporated i.V., the residue was dissolved in MeCl2 and water, the pH was adjusted to ˜10 with sodium carbonate solution and the mixture was extracted twice with MeCl2; the organic phases were washed with water, dried over MgSO4, filtered and evaporated i.V. The crude product was purified by chromatography (silicagel, eluent:gradient of MeCl2/MeOH) to yield 1.20 g of the title compound as colorless oil. MS: 335.2 (MH+).

1. customThen, the reaction mixture was evaporated i.V
2. dissolution, the residue was dissolved in MeCl2
3. extractionthe mixture was extracted twice with MeCl2
4. washthe organic phases were washed with water
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated i.V
8. customThe crude product was purified by chromatography (silicagel, eluent:gradient of MeCl2/MeOH)