Iodine → HCID 14743030, 화합물

HRID 747693

반응식

HRID 747693 반응식
[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

참가 물질

7

반응물 5

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

생성물 1

HCID 14743030HCID 14743030, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cbdd96963f104d08869b85dddfa470eb
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07396844B1

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