Potassium Iodide → HCID 178524773, 화합물

HRID 488462

반응식

HRID 488462 반응식
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.[I:11]([O-])(=O)=O.[K+].[I-].[K+]>O.OS(O)(=O)=O>[OH:1][C:2]1[C:10]([I:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1

참가 물질

6

반응물 3

HCID 4875Potassium IodideHCID 23665710Potassium IodateHCID 178418479HCID 178418479, 화합물

생성물 1

HCID 178524773HCID 178524773, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1118Sulfuric Acid용매

반응 조건

온도
60 °C

실험 절차

6-Hydroxynicotinic acid (20 g) in water (200 ml) and H2SO4 (80 ml) was heated to 90° C. for 1 hour. Potassium iodate (0.42 equivalent) and potassium iodide (0.96 equivalent) were both added portionwise over 2 hours. After a further hour at 90° C. the mixture was cooled to 60° C. and added to 1 kg of ice. The brown solid was filtered off, dried and taken up in DMF (30 ml)/EtOH(1 litre). Sodium metabisulfite was added until the brown colour disappeared and the mixture was poured onto ice (2 kg), a further 1.5 litre water added and the white solid filtered to give title compound (16.5 g). NMR δ(DMSO) 12.95 (1H, broad), 12.35 (1H, broad), 8.36 (1H, d), 8.03 (1H, d)

후처리

  1. additionboth added portionwise over 2 hours
  2. filtrationThe brown solid was filtered off
  3. customdried
  4. additionSodium metabisulfite was added until the brown colour
  5. additionthe mixture was poured onto ice (2 kg)
  6. additiona further 1.5 litre water added
  7. filtrationthe white solid filtered

출처 및 근거

ORD 기록
ord-4d1cf850ac544cdda7fec36221f94862
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06972297B2

연결된 노트

불러오는 중…