Iodine → 5-Iodo-3-methylpyridin-2-amine

HRID 226355

반응식

HRID 226355 반응식
[CH3:1][C:2]1[C:3]([NH2:8])=[N:4][CH:5]=[CH:6][CH:7]=1.S(=O)(=O)(O)O.[I:14](O)(=O)(=O)=O.II.[O-]S([O-])(=S)=O.[Na+].[Na+]>O.CC(O)=O>[I:14][C:6]1[CH:7]=[C:2]([CH3:1])[C:3]([NH2:8])=[N:4][CH:5]=1

참가 물질

8

반응물 5

HCID 807IodineHCID 1118Sulfuric AcidHCID 153472-Amino-3-methylpyridineHCID 24477Sodium ThiosulfateHCID 65185Metaperiodic acid

생성물 1

HCID 9595865-Iodo-3-methylpyridin-2-amine수율 174.9%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

To a solution of 3-methyl-2-pyridineamine (10 g) in a mixed solution of AcOH (60 mL), water (12 mL), and sulfuric acid (4.2 mL) was added periodic acid dehydrate (4.22 g) and iodine (9.39 g), and the mixture was heated at 80° C. for 2 hours. The reaction mixture was poured into 5% Na2S2O3 aq solution and extracted with ether. The organic layer was washed with 1N NaOH aq solution and brine, and dried over Na2SO4. The solvent was removed in vacuo and obtained residual solid was recrystallized with EtOH to give 5-iodo-3-methyl-2-pyridinamine (9.00 g) as pale yellow powder.

후처리

  1. extractionextracted with ether
  2. washThe organic layer was washed with 1N NaOH aq solution and brine
  3. dry with materialdried over Na2SO4
  4. customThe solvent was removed in vacuo
  5. customobtained residual solid
  6. customwas recrystallized with EtOH

출처 및 근거

ORD 기록
ord-53f55ca96c1d4c3cab9aef891b414de3
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557127B2

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