Sodium Iodide → 3-(2-Cyanophenyl)-5-(2-pyridyl)-2(1H)-pyridone

HRID 497820ノート

反応式

HRID 497820 の反応式
Cl[Si](C)(C)C.[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[C:15]([O:26]C)=[N:16][CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[CH:19]=1)#[N:7].[I-].[Na+].C(=O)(O)[O-].[Na+]>C(#N)C>[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[C:15](=[O:26])[NH:16][CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[CH:19]=1)#[N:7]

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 516892Sodium BicarbonateHCID 223190893-(2-Cyanophenyl)-5-(2-pyridyl)-2-methoxypyridine

生成物 1

HCID 223189453-(2-Cyanophenyl)-5-(2-pyridyl)-2(1H)-pyridone収率 57.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Chlorotrimethylsilane (0.1 ml) was added to a suspension of 0.20 g of 3-(2-cyanophenyl)-5-(2-pyridyl)-2-methoxypyridine and 0.12 g of sodium iodide in 10 ml of acetonitrile and the mixture was stirred at room temperature for 3 hours. A saturated sodium bicarbonate solution was added to the mixture followed by extracting with ethyl acetate. The ethyl acetate layer was washed with water and a saturated saline solution and dried over magnesium sulfate. The solvent was concentrated in vacuo and the residue was purified by a silica gel column chromatography (ethyl acetate:hexane=1:1) to give 0.11 g of the title compound in pale yellow powder.

後処理

  1. extractionby extracting with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materiala saturated saline solution and dried over magnesium sulfate
  4. concentrationThe solvent was concentrated in vacuo
  5. customthe residue was purified by a silica gel column chromatography (ethyl acetate:hexane=1:1)

出典と根拠

ORDレコード
ord-c2af947a0957471ab4a94c83f76b3ff1
出典データセット
uspto-grants-2005_09
特許番号
US06949571B2

反応ノート

読み込み中…