反应详情

767 mg (3.15 mmol) 1-(2,2,2-trifluoroacetyl)piperidine-4-carboxylic acid chloride dissolved in CH2Cl2 was slowly added drop-wise to 526 mg (2.10 mmol) 3-amino-6-bromo-1H-indole-2-carboxylic acid amide (Example 4) in pyridine at 0° C. Then, stirring was carried out at room temperature for 40 min. After the addition of water, the solvent was removed in vacuo and the residue was taken up in methanol. After the addition of 2 M NaOH (excess), the reaction was kept at reflux for 45 min. Thereafter, the methanol was removed in vacuo, the precipitate was sucked off and washed with water. 652 mg (89%) 7-bromo-2-(4-piperidyl)-5H-pyrimido[5,4-b]indol-4-ol was obtained. ESI-MS [m/z]: 347, 349 [M+H]+

1. customat 0° C
2. customthe solvent was removed in vacuo
3. additionAfter the addition of 2 M NaOH (excess)
4. temperatureat reflux for 45 min
5. customThereafter, the methanol was removed in vacuo
6. washwashed with water