반응 #157309

ord-19e6337ddada4661bb84eebb88a950a1

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to reflux overnight
  2. 2
    농축the reaction mixture was concentrated under reduced pressure
  3. 3
    여과collected by filtration
  4. 4
    세척washed with water (2×)
  5. 5
    기타air-dried
  6. 6
    기타Further drying in a 35° C. vacuum oven

실험 절차

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

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822472B2uspto-grants-2014_09