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Methyl iodide → 1-Methoxy-4-(2-methyl-2-nitropropyl)benzene

HRID 2172707
ノート
印刷プレビュー

反応式

HRID 2172707 の反応式
IC.[CH3:3][C:4]([N+:14]([O-:16])=[O:15])([CH3:13])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1.[C:17](=O)([O-])[O-].[K+].[K+]>O1CCCC1.CN(C)C=O>[CH3:17][O:12][C:9]1[CH:10]=[CH:11][C:6]([CH2:5][C:4]([CH3:3])([N+:14]([O-:16])=[O:15])[CH3:13])=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 128269024-(2-Methyl-2-nitropropyl)phenol

生成物 1

HCID 128269081-Methoxy-4-(2-methyl-2-nitropropyl)benzene収率 63.7%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran
溶媒

実験手順

Iodomethane (0.12 mL, 1.3 mmol) was added to a mixture of 4-(2-methyl -2-nitropropyl)phenol (300 mg, 1.5 mmol) and potassium carbonate (425 mg, 3.1 mmol) in tetrahydrofuran (20 mL) and N,N-dimethylformamide (1 mL). After refluxing overnight, the mixture was cooled and concentrated under vacuum. The residue was dissolved in ethyl acetate, washed with water, dried over anhydrous sodium sulfate and concentrated to provide crude 1-methoxy-4-(2-methyl-2-nitropropyl)benzene (200 mg, 62% yield) as yellow oil which was used directly in the next step.

後処理

  1. temperatureAfter refluxing overnight
  2. temperaturethe mixture was cooled
  3. concentrationconcentrated under vacuum
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-3e07d6589cf8436fa8b93656b0c68c90
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09056852B2

反応ノート

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