반응 #2507847

반응 방정식

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

용매

ethyl acetate

dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added in portions
2. 2
   기타was back to ambient temperature
3. 3
   세척The organic phase was washed with aqueous saturated sodium chloride
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   농축concentrated

실험 절차

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%)

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