反应详情

温度

0 °C

(2S)-1-(2-(N-tert-Butyloxycarbonyl-N-(2-methylpropyl)amino)acetyl)pyrrolidine-2-carbonitrile (25 mg, 0.081 mmol) was treated with trifluoroacetic acid (50 ml). After 1 h at room temperature the solvent was removed in vacuo and the residue dissolved in CH2Cl2 (100 ml). The solution was cooled to 0° C., triethylamine (30 mg, 0.3 mmol) was added followed by 2-anisoyl chloride (15 mg, 0.088 mmol). After 18 h at 0° C. to room temperature the solvent was removed in vacuo and the residue dissolved in ethyl acetate (200 ml). This solution was washed with 0.3M KHSO4, sat. NaHCO3, water and brine, dried (Na2SO4) and evaporated in vacuo. The residue was purified by flash chromatography (eluant: 2% methanol, 98% chloroform) to give a colourless oil identified as the title compound (18 mg, 0.052 mmol, 66%).

1. customAfter 1 h at room temperature the solvent was removed in vacuo
2. dissolutionthe residue dissolved in CH2Cl2 (100 ml)
3. customAfter 18 h at 0° C. to room temperature the solvent was removed in vacuo
4. dissolutionthe residue dissolved in ethyl acetate (200 ml)
5. washThis solution was washed with 0.3M KHSO4, sat. NaHCO3, water and brine
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customThe residue was purified by flash chromatography (eluant: 2% methanol, 98% chloroform)
9. customto give a colourless oil