反应详情

To a stirred solution of 4-{N′-[2-(4-fluoro-phenyl)-acetyl]-N′-methyl-hydrazino}-piperidine-1-carboxylic acid tert-butyl ester, 9, (3.7 g, 10.1 mmol) in pyridine (10 mL) is added 2-methylsulfanyl-pyrimidine-4-carbonyl chloride (2.9 g, 15.2 mmol). The reaction mixture is stirred at room temperature for 2 hours then diluted with 0.1 N HCl and extracted three times with CH2Cl2. The combined organic layers are dried (MgSO4), filtered and concentrated in vacuo. Purification over silica (EtOAc/hexanes 1:1) affords 1.058 g (20% yield) of the desired product. ESI/MS: 518.2 (M+H).

1. extractionextracted three times with CH2Cl2
2. dry with materialThe combined organic layers are dried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customPurification over silica (EtOAc/hexanes 1:1)