反应详情

温度

90 °C

10.0 mg of 1H-pyrazole-3-carboxaldehyde was added to an N,N-dimethylformamide (1 ml) solution of 49.0 mg of t-butyl 2-(4,5-diamino-2-(4-methanesulfonyl-phenoxy)-phenyl)-pyrrolidine-1-carboxylate obtained in Example 306 (step 3), and the reaction liquid was stirred overnight at 90° C. After cooled, the reaction liquid was diluted with ethyl acetate, washed with saturated saline, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=9/1) to obtain the entitled compound as a brown solid.

1. customthe reaction liquid
2. temperatureAfter cooled
3. customthe reaction liquid
4. washwashed with saturated saline
5. dry with materialdried with anhydrous magnesium sulfate
6. customThe solvent was evaporated away under reduced pressure
7. customthe resulting residue was purified
8. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=9/1)