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Iodine → 2-Chloro-3-iodopyridin-4-amine

HRID 536205
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인쇄 미리보기

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HRID 536205 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-:15].[K+].II.[OH-].[Na+].S([O-])([O-])(=O)=S.[Na+].[Na+]>O>[Cl:1][C:2]1[C:7]([I:15])=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 807IodineHCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 24477Sodium ThiosulfateHCID 844322-Chloropyridin-4-amine

생성물 1

HCID 242292082-Chloro-3-iodopyridin-4-amine수율 19.6%

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온도
100 °C

실험 절차

Commercially available 2-chloro-4-aminopyridine (15 g, 0.1 mol) and 37.2 g (0.4 mol) of sodium carbonate are suspended in 200 ml of water and warmed to 100° C. 58.3 g (0.4 mol) of potassium iodide and 59.4 g (0.2 mol) of iodine are added to the resultant solution, and the mixture is stirred at the temperature indicated for 12 h. The mixture is subsequently adjusted to pH 13 using sodium hydroxide solution, treated with sodium thiosulfate until completely decolorised and extracted with ethyl acetate. Chromatographic purification gives 5 g (17%) of solid.

후처리

  1. extractionextracted with ethyl acetate
  2. customChromatographic purification

출처 및 근거

ORD 기록
ord-a5e1bc3944384b66943ecd4470c3c552
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859581B2

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시약·촉매·용매 1

HCID 962Water용매