Iodine → HCID 14743030、化合物

HRID 747693

反応式

HRID 747693 の反応式
[CH2:1]([C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(=O)(=O)(O)O.II.[I:21]([O-])(=O)=O.[Na+].I([O-])(=O)(=O)=O.[Na+]>C(O)(=O)C>[I:21][C:5]1[CH:4]=[CH:3][C:2]([CH2:1][C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)=[CH:7][CH:6]=1

参加物

7

反応物 5

HCID 807IodineHCID 1118Sulfuric AcidHCID 164584-BenzylpyridineHCID 23667635Sodium periodateHCID 23675764Sodium Iodate

生成物 1

HCID 14743030HCID 14743030、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

5.0 g (30 mmol) of 4-benzylpyridine was dissolved in 30 ml of acetic acid. 3.53 ml (65 mmol) of concentrated sulfuric acid, 2.99 g (11.8 mmol) of iodine and 1.17 g (5.9 mmol) of sodium iodate were added to the solution, and the resultant mixture was stirred at 70° C. for 20 hours. After cooling, 0.15 g of sodium metaperiodate was added to the reaction mixture. After the distillation under reduced pressure, water was added to the residue, which was washed with dichloromethane. After the addition of 1 N aqueous sodium hydroxide solution followed by the extraction with dichloromethane twice, the solvent was evaporated. The residue was purified by the silica gel column chromatography to obtain the title compound.

後処理

  1. temperatureAfter cooling
  2. distillationAfter the distillation under reduced pressure, water
  3. additionwas added to the residue, which
  4. washwas washed with dichloromethane
  5. additionAfter the addition of 1 N aqueous sodium hydroxide solution
  6. extractionfollowed by the extraction with dichloromethane twice
  7. customthe solvent was evaporated
  8. customThe residue was purified by the silica gel column chromatography

出典と根拠

ORDレコード
ord-cbdd96963f104d08869b85dddfa470eb
出典データセット
uspto-grants-2008_07
特許番号
US07396844B1

関連ノート

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