تفاعل #3876

ord-dedcc622a9794abe8181ef0f7412474d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04722934uspto-grants-1988_02