反应详情

温度

0 °C

To a solution of 4-{N′-[2-(4-fluoro-phenyl)-acetyl]-N′-methyl-N-(2-methylsulfanyl-pyrimidine-4-carbonyl)-hydrazino}-piperidine-1-carboxylic acid tert-butyl ester, 10, (1.058 g, 2.05 mmol) in DMF (2 mL) at 0° C. is slowly added NaH (123 mg of a 60% dispersion in mineral oil, 3.07 mmol). The reaction mixture is stirred for 1 hour at 0° C. and then quenched with 0.1 N HCl. The aqueous layer is extracted three times with CH2Cl2 and the combined organic layers are dried (MgSO4), filtered and concentrated in vacuo. Purification over silica (20% MeOH/CHCl3) affords 0.743 g (73% yield) of the diesired product. ESI/MS: 500.2 (M+H).

1. customat 0° C.
2. customquenched with 0.1 N HCl
3. extractionThe aqueous layer is extracted three times with CH2Cl2
4. dry with materialthe combined organic layers are dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification over silica (20% MeOH/CHCl3)