反应详情

温度

65 °C

small screw cap test tube was charged with 2,5-Dimethyl-2H-pyrazole-3-carboxylic acid [3-(3-hydroxymethylene-2-oxo-2,3-dihydro-1H-indole-6-carbonyl)-phenyl]-amide (as prepared in Example 60, 200 mg, 0.498 mmol) and THF (4 mL). To the resulting solution was added 4-[(2-Pyrrolidin-1-yl-ethylamino)-methyl]-phenylamine (prepared below; 109.2 mg, 0.498 mmol), and the mixture was stirred for 24 h at 65° C. The reaction mixture was cooled to room temperature. Hexanes were added to the reaction mixture causing a black precipitate to form. The precipitate was vacuum filtered and the filtrate was then concentrated in vacuo and redissolved into ˜5 mL of EtOAc. Hexanes were added causing a yellow precipitate to form. The precipitate was then filtered and washed with ˜1 mL of i-prOH yielding 31% (0.092 g, 0.152 mmol) of the title compound.

1. customsmall screw cap test tube
2. temperatureThe reaction mixture was cooled to room temperature
3. customto form
4. filtrationfiltered
5. concentrationthe filtrate was then concentrated in vacuo
6. dissolutionredissolved into ˜5 mL of EtOAc
7. additionHexanes were added
8. customto form
9. filtrationThe precipitate was then filtered