反应详情

温度

0 °C

A mixture of 4-[2-(6-methyl-pyridin-2-yl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]-quinoline-7-carboxylic acid(2-amino-1,1-dimethyl-ethyl)-amide (0.12 g, 0.27 mmol), sodium cyanoborohydride (0.038 g, 0.6 mmol), and acetic acid (0.077 mL, 1.3 mmol) in methanol (5 mL) is cooled to 0° C. and stirred for 10 min. A solution of 37% aqueous formaldehyde (0.086 mL, 3.1 mmol) in methanol (2 mL) is added dropwise. The mixture is allowed to warm to room temperature and stirred for 1 h. The reaction is quenched with saturated aqueous potassium carbonate solution and concentrated in vacuo. The residue is taken up in chloroform, washed with water and brine, dried (sodium sulfate) and concentrated in vacuo. The residue is chromatographed on SiO2 (8% methanol/92% dichloromethane) to yield the title compound, 33 mg (27%), as a white foam.

1. temperatureto warm to room temperature
2. stirringstirred for 1 h
3. customThe reaction is quenched with saturated aqueous potassium carbonate solution
4. concentrationconcentrated in vacuo
5. washwashed with water and brine
6. dry with materialdried (sodium sulfate)
7. concentrationconcentrated in vacuo
8. customThe residue is chromatographed on SiO2 (8% methanol/92% dichloromethane)