反应详情

391 mg (0.91 mmol) of N-ethyl-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyrimidin-2-amine were dissolved in a mixture of 20 ml of dioxane and 4 ml of water. 239 mg (3.64 mmol) of metallic zinc and 485 mg (9.1 mmol) of ammonium chloride were then added to the resulting solution. The reaction was carried out at 100° C. under stirring for 5 hours. The suspension was then filtered through a celite pad and the filtrate evaporated in vacuo. The residue was partitioned between dichloromethane and aqueous sodium hydrogenocarbonate and the organic layer dried over sodium sulphate and concentrated to give a crude purified by flash-chromatography on a silica gel column (CH2Cl2-CH3COCH3; from 9/1 to 7/3), affording 340 mg (93%) of the title compound.

1. customwas carried out at 100° C.
2. filtrationThe suspension was then filtered through a celite pad
3. customthe filtrate evaporated in vacuo
4. customThe residue was partitioned between dichloromethane and aqueous sodium hydrogenocarbonate
5. dry with materialthe organic layer dried over sodium sulphate
6. concentrationconcentrated
7. customto give a crude
8. custompurified by flash-chromatography on a silica gel column (CH2Cl2-CH3COCH3; from 9/1 to 7/3)