تفاعل #157309

ord-19e6337ddada4661bb84eebb88a950a1

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto reflux overnight
  2. 2
    تركيزthe reaction mixture was concentrated under reduced pressure
  3. 3
    ترشيحcollected by filtration
  4. 4
    غسيلwashed with water (2×)
  5. 5
    أخرىair-dried
  6. 6
    أخرىFurther drying in a 35° C. vacuum oven

الإجراء التجريبي

3-Hydroxy-2-aminopyridine (2.00 g, 18.2 mmol) and potassium hydroxide (1.22 g, 21.8 mmol) were dissolved in carbon disulfide (15 mL) and EtOH (25 mL), and the reaction mixture was heated to reflux overnight. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The resulting solid was suspended in 1 M aqueous HCl, collected by filtration, washed with water (2×) and air-dried. Further drying in a 35° C. vacuum oven gave 2.52 g (91%) of the title compound as a tan solid. LC-MS: RT=4.82 min., [M+H]+=153.1

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08822472B2uspto-grants-2014_09