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Iodine → 2-Amino-5-chloro-3-iodopyridine

HRID 58651
ノート
印刷プレビュー

反応式

HRID 58651 の反応式
[I:1]I.[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([NH2:10])=[N:8][CH:9]=1>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[Cl:3][C:4]1[CH:5]=[C:6]([I:1])[C:7]([NH2:10])=[N:8][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 807IodineHCID 661742-Amino-5-chloropyridine

生成物 1

HCID 110760102-Amino-5-chloro-3-iodopyridine収率 64%

試薬・触媒・溶媒 2

HCID 178418844HCID 178418844、化合物触媒HCID 702Ethanol溶媒

実験手順

Iodine (7.55 g; 29.73 mmol) was added to a mixture of 5-chloropyridin-2-amine (3.00 g; 22.87 mmol) and silver sulphate (9.36 g; 29.73 mmol) in ethanol (150 mL) and the mixture was stirred overnight at room temperature. The mixture was filtered over celite, washed with ethanol, and the filtrate concentrated under reduced pressure. The residue was dissolved in dichloromethane, and the solution was washed with a saturated aqueous solution of sodium thiosulphate. The organic layer was dried over magnesium sulphate, concentrated under reduced pressure and the crude material purified by flash chromatography on silica gel (eluent: 0 to 30% of ethyl acetate in heptane) to give 3.71 g (64%) of 5-chloro-3-iodopyridin-2-amine as a beige solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. filtrationThe mixture was filtered over celite
  2. washwashed with ethanol
  3. concentrationthe filtrate concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in dichloromethane
  5. washthe solution was washed with a saturated aqueous solution of sodium thiosulphate
  6. dry with materialThe organic layer was dried over magnesium sulphate
  7. concentrationconcentrated under reduced pressure
  8. customthe crude material purified by flash chromatography on silica gel (eluent: 0 to 30% of ethyl acetate in heptane)

出典と根拠

ORDレコード
ord-601e897bc3144f69904f9d03319b7ee7
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434722B2

反応ノート

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