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

HRID 1994229
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HRID 1994229 반응식
[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]
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참가 물질

5

반응물 3

HCID 10962Butyl iodideHCID 14797Potassium HydroxideHCID 22266504HCID 22266504, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
85 °C

실험 절차

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%).

후처리

  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))

출처 및 근거

ORD 기록
ord-1727cd7306414d7c9253bca6d1df2170
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652141B2

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