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Butyl iodide → 1-Butyl-5,6-dimethyl-3-methoxy-2-pyridone

HRID 416546
ノート
印刷プレビュー

反応式

HRID 416546 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([O:10][CH3:11])[C:5](=[O:9])[NH:6][C:7]=1[CH3:8].[OH-].[K+].I[CH2:15][CH2:16][CH2:17][CH3:18]>C(O)CCC>[CH2:15]([N:6]1[C:7]([CH3:8])=[C:2]([CH3:1])[CH:3]=[C:4]([O:10][CH3:11])[C:5]1=[O:9])[CH2:16][CH2:17][CH3:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10962Butyl iodideHCID 14797Potassium HydroxideHCID 22266504HCID 22266504、化合物

生成物 1

HCID 222665381-Butyl-5,6-dimethyl-3-methoxy-2-pyridone収率 29.6%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
85 °C

実験手順

n-Butanol (13 mL) was added to a mixture of 5,6-dimethyl-3-methoxy-2-pyridone (1-004-06) (306 mg) and potassium hydroxide (157 mg). 1-Iodobutane (0.44 mL) was added to the suspension, and the reaction mixture was heated with stirring in an oil bath at 85° C. under nitrogen atmosphere. After 24 h, the reaction mixture was evaporated under reduced pressure, and the residue was dissolved in acetyl acetate and water. The reaction mixture was extracted twice with ethyl acetate, and once with water, dried over magnesium sulfate, and evaporated under reduced pressure. The obtained residue (300 mg) was purified by silica gel column chromatography (Lobar column B, toluene/acetone (3/1)) to give 1-butyl-5,6-dimethyl-3-methoxy-2-pyridone (1-004-07) (124 mg, 29.6%).

後処理

  1. temperaturethe reaction mixture was heated
  2. customthe reaction mixture was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in acetyl acetate
  4. extractionThe reaction mixture was extracted twice with ethyl acetate
  5. dry with materialonce with water, dried over magnesium sulfate
  6. customevaporated under reduced pressure
  7. customThe obtained residue (300 mg) was purified by silica gel column chromatography (Lobar column B, toluene/acetone (3/1))

出典と根拠

ORDレコード
ord-f391c593008c49f19914eda53218d2a8
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08088924B2

反応ノート

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