反应详情

温度

0 °C

0.95 g (2.2 mmol) of (S)-N-(α-ethylbenzyl)-3-(2-aminoethoxy)-2-phenylquinoline-4-carboxamide (compound of Description 4) were dissolved, under nitrogen atmosphere and magnetical stirring, in 12 ml of dry CH2Cl2; 0.37 ml (2.6 mmol) of TEA were added, the solution cooled to 0° C. and 0.3 ml (2.6 mmol) of benzoyl chloride, dissolved in in 3 ml dry CH2Cl2 were added dropwise. The reaction was left 30 minutes at 0° C., then allowed to reach room temperature and left overnight. The mixture was evaporated in-vacuo to dryness, the residue was dissolved in CH2Cl2, and washed with H2O, 20% citric acid, sat. sol. NaHCO3, sat. sol. NaCl; the organic layer was dried over Na2SO4 and evaporated in-vacuo to dryness. The residue was triturated with hot i-Pr2O/i-PrOH to yield 0.8 g of the title compound as a white solid.

1. additionwere added dropwise
2. customto reach room temperature
3. waitleft overnight
4. customThe mixture was evaporated in-vacuo to dryness
5. dissolutionthe residue was dissolved in CH2Cl2
6. washwashed with H2O, 20% citric acid, sat. sol. NaHCO3, sat. sol. NaCl
7. dry with materialthe organic layer was dried over Na2SO4
8. customevaporated in-vacuo to dryness
9. customThe residue was triturated with hot i-Pr2O/i-PrOH