تفاعل #54397

ord-3e22b618bac643c9a551629a270f7fb7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated on the steam bath a total of six hours
  2. 2
    درجة الحرارةAfter a few minutes of heating
  3. 3
    درجة الحرارةThe mixture was cooled somewhat
  4. 4
    أخرىthe orange solid was isolated by suction filtration
  5. 5
    غسيلAfter washing once with tetrahydrofuran, twice with ether
  6. 6
    أخرىdrying

الإجراء التجريبي

41.0 g (0.10 mole) of 4,4-dibromo-3-methyl-1-(4-sulfophenyl)-2-pyrazolin-5-one, which can be prepared according to the method of Machiele, U.S. Pat. No. 3,952,009 (Example 1), and 16.0 g (0.15 mole) of 2-hydrazinopyridine were combined in 180 ml of water. The mixture was heated on the steam bath a total of six hours. After a few minutes of heating, the solution goes to a very thick slurry. The mixture was cooled somewhat, 10 ml of concentrated HCl were added, and the orange solid was isolated by suction filtration. After washing once with tetrahydrofuran, twice with ether, and drying, the yield of dye was 17.8 g (50 percent).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04148641uspto-grants-1979_04