反应详情

温度

65 °C

A 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, 100 mg, 0.249 mmol) and THF (2.5 mL). To the resulting solution was added N-(2-Morpholin-4-yl-ethyl)-benzene-1,4-diamine (prepared below, 77.1 mg, 0.348 mmol), and the mixture was stirred for 24 h at 65° C. The reaction mixture was cooled to room temperature and then diluted with Hexanes (˜40 mL). The black precipitate that formed was removed by filtration and the filtrate was concentrated in vacuo. The crude residue was dissolved in EtOAc (˜5 mL) and triturated with Hexane (˜50 mL) to give a yellow precipitate. The precipitate was filtered and washed with 0° C. i-prOH (˜5 mL) yielding 45% (0.0677 g, 0.112 mmol) of the title compound.

1. customA small screw cap test tube
2. temperatureThe reaction mixture was cooled to room temperature
3. customThe black precipitate that formed
4. customwas removed by filtration
5. concentrationthe filtrate was concentrated in vacuo
6. dissolutionThe crude residue was dissolved in EtOAc (˜5 mL)
7. customtriturated with Hexane (˜50 mL)
8. customto give a yellow precipitate
9. filtrationThe precipitate was filtered
10. washwashed with 0° C.