تفاعل #81819

ord-f41d23391e474101991fe6e5a3777f55

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwarmed to 60° C. for 5 minutes
  2. 2
    درجة الحرارةAfter cooling to room temperature the mixture
  3. 3
    استخلاصThe mixture was extracted with chloroform (3×30 mL)
  4. 4
    غسيلThe combined organic phase was washed
  5. 5
    أخرىdried
  6. 6
    أخرىevaporated

الإجراء التجريبي

To a suspension of 2-chloro-3-cyano-6-(N,N-dimethylamino)-4-methylpyridine (0.98 g) in acetic acid (10 mL) was added bromine (0.9 g) in acetic acid (1 mL). The reaction mixture was stirred at room temperature for 20 minutes and then warmed to 60° C. for 5 minutes. After cooling to room temperature the mixture was poured into a solution of sodium hydroxide (8 g) in water (100 mL). The mixture was extracted with chloroform (3×30 mL). The combined organic phase was washed, dried, and evaporated to give 1.36 g of the title compound, suitable for use in the next reaction.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05620974uspto-grants-1997_04