反应 #2507847

反应方程式

1,2-Dihydro-4-((4-ethylphenyl)methyl)-5-(trifluoromethyl)-3H-pyrazol-3-one

t-Butyldimethylsilyl chloride

Water

imidazole

→

desired compound

3-t-butyldimethylsilyloxy-4-((4-ethylphenyl)methyl)-5-(trifluoromethyl)-1H-pyrazole

溶剂

ethyl acetate

dimethylformamide

反应条件

后处理

1. 1
   workup.ADDITIONwas added in portions
2. 2
   其他was back to ambient temperature
3. 3
   洗涤The organic phase was washed with aqueous saturated sodium chloride
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   浓缩concentrated

实验过程

1,2-Dihydro-4-((4-ethylphenyl)methyl)-5-(trifluoromethyl)-3H-pyrazol-3-one (4) (prepared by the method described in J. Med. Chem 1996, 39, 3920-3928) (15.0 g; 55.6 mmol) was dissolved in dimethylformamide (150 ml) and cooled to 0° C. t-Butyldimethylsilyl chloride (9.3 g; 61.1 mmol) was added in portions, and then, imidazole (4.2 g; 61.1 mmol) was added in portions. Then, the resulting mixture was back to ambient temperature, then the mixture was stirred for 3 hours. Water was added to the reaction solution, for extraction twice with ethyl acetate. The organic phase was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, to give the desired compound (21.4 g; 55.6 mmol). (100%)

来源