Ethylene Glycol → HCID 86643578、化合物

HRID 1848957ノート

反応式

HRID 1848957 の反応式
[Cl:1][C:2]1[C:7](I)=[C:6]([NH2:9])[CH:5]=[CH:4][N:3]=1.[C:10]1([SH:16])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(O)CO.C(=O)([O-])[O-].[K+].[K+]>[Cu]I.C(O)(C)C>[Cl:1][C:2]1[C:7]([S:16][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[C:6]([NH2:9])[CH:5]=[CH:4][N:3]=1

参加物

7

反応物 4

HCID 174Ethylene GlycolHCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 242292082-Chloro-3-iodopyridin-4-amine

生成物 1

HCID 86643578HCID 86643578、化合物収率 91%

試薬・触媒・溶媒 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 3776Isopropanol溶媒

実験手順

To a 250 mL round flask was added 2-chloro-3-iodo-4-aminopyridine (5.0 g, 19.6 mmol), thiophenol (2.16 g, 19.6 mmol), CuI (0.187 g, 0.98 mmol), ethylene glycol (2.5 g, 39 mmol), potassium carbonate (5.4 g, 39 mmol), and 150 mL of isopropanol. The reaction was heated to reflux and stirred under a nitrogen atmosphere for 24 h. After cooling, the mixture was purified by a silica gel column. Yield (91%) of 2-chloro-3-phenylthio-4-aminopyridine was 4.2 g.

後処理

  1. temperatureThe reaction was heated
  2. temperatureto reflux
  3. temperatureAfter cooling
  4. customthe mixture was purified by a silica gel column

出典と根拠

ORDレコード
ord-c72578119b7f424d89ee276df3a1e5cd
出典データセット
uspto-grants-2015_02
特許番号
US08952363B2

反応ノート

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