Potassium Iodide → HCID 178524773、化合物

HRID 488462

反応式

HRID 488462 の反応式
[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

参加物

6

反応物 3

HCID 4875Potassium IodideHCID 23665710Potassium IodateHCID 178418479HCID 178418479、化合物

生成物 1

HCID 178524773HCID 178524773、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒

反応条件

温度
60 °C

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-4d1cf850ac544cdda7fec36221f94862
出典データセット
uspto-grants-2005_12
特許番号
US06972297B2

関連ノート

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