반응 #3876

반응 방정식

3-[2-[4-(4-trifluoromethylphenoxy)phenoxy]-propionyl]-thiocarbazic acid-O-ethyl ester

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compound

수율 57.4%

2-ethoxy-5-[1-[4-(4-trifluoromethylphenoxy)phenoxy]-ethyl]-1,3,4-thiadiazole

수율 57.4%

용매

sulfuric acid

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGAfter stirring at the same temperature for 10 minutes
3. 3
   추출by extracting with ethyl acetate
4. 4
   세척The resulting ethyl acetate layer was washed with water
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   농축concentrated
7. 7
   기타The residue was purified by chromatography on silica gel

실험 절차

To 10 ml of concentrated sulfuric acid cooled to -5° C. was added, with stirring, 2.0 g of 3-[2-[4-(4-trifluoromethylphenoxy)phenoxy]-propionyl]-thiocarbazic acid-O-ethyl ester gradually. After stirring at the same temperature for 10 minutes, the reaction mixture was poured over 100 g of ice followed by extracting with ethyl acetate. The resulting ethyl acetate layer was washed with water, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by chromatography on silica gel to obtain 1.1 g of the compound No. 5 described in Table 1.

출처