Potassium Iodide → HCID 58351061、化合物

HRID 475719ノート

反応式

HRID 475719 の反応式
[Br:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([NH:10][CH:11]=[O:12])=[CH:4][CH:3]=1.[I-].[K+].C(=O)([O-])[O-].[Cs+].[Cs+].Cl[CH2:22][C:23](=[O:25])[CH3:24]>CN(C=O)C>[Br:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([N:10]([CH2:22][C:23](=[O:25])[CH3:24])[CH:11]=[O:12])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 6571ChloroacetoneHCID 10796Cesium carbonateHCID 71492501N-(6-bromo-2-methoxypyridin-3-yl)formamide

生成物 1

HCID 58351061HCID 58351061、化合物収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of N-(6-bromo-2-methoxypyridin-3-yl)formamide (5.69 g, 24.63 mmol), potassium iodide (0.450 g, 2.71 mmol) and cesium carbonate (28.1 g, 86 mmol) in 66 mL of DMF was added 1-chloropropan-2-one (4.90 mL, 61.6 mmol). The reaction mixture was stirred at rt for 3 days. The reaction mixture was poured into icewater and extracted with ethyl acetate. The combined organic extracts were dried over anhydrous magnesium sulfate and filtered. The solvent was removed in vacuum to give N-(6-bromo-2-methoxypyridin-3-yl)-N-(2-oxopropyl)formamide (7.07 g, 24.62 mmol, 100% yield) as brown solid. LC-MS (M+Na)+=310.9.

後処理

  1. additionThe reaction mixture was poured into icewater
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was removed in vacuum

出典と根拠

ORDレコード
ord-75212d285d6b49569884e2ad8fda0dcc
出典データセット
uspto-grants-2014_01
特許番号
US08637525B2

反応ノート

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