反应详情

温度

60 °C

Add lithium aluminum hydride (210 mg, 5.5 mmol) portionwise over 3 min to a solution of 4-[2-(3-methyl-butylamino)-thiazol-4-yl]-benzonitrile (500 mg, 1.8 mmol) in THF (20 mL) at room temperature under a nitrogen atmosphere. Stir the mixture for 1 h at 60° C. Cool the mixture, quench slowly with water (0.2 mL) and 1N NaOH (0.2 mL). Add sodium sulfate to absorb residual water, filter the mixture through Celite®, wash with DCM (50 mL) and concentrate in vacuo. Purify the residue by SCX chromatography to obtain the desired intermediate (493 mg, 97%). MS (ES+) m/z: 276 (M+H)+.

1. temperatureCool the mixture
2. customquench slowly with water (0.2 mL) and 1N NaOH (0.2 mL)
3. customAdd sodium sulfate to absorb residual water
4. filtrationfilter the mixture through Celite®
5. washwash with DCM (50 mL)
6. concentrationconcentrate in vacuo
7. customPurify the residue by SCX chromatography