Methyl iodide → 4-(2,2,2-Trifluoro-1-methoxyethyl)pyridine-2-carbonitrile

HRID 1880764ノート

反応式

HRID 1880764 の反応式
[F:1][C:2]([F:14])([F:13])[CH:3]([C:5]1[CH:10]=[CH:9][N:8]=[C:7]([C:11]#[N:12])[CH:6]=1)[OH:4].[C:15](=O)([O-])[O-].[K+].[K+].CI.[Cl-].[NH4+]>CN(C)C=O>[F:14][C:2]([F:1])([F:13])[CH:3]([C:5]1[CH:10]=[CH:9][N:8]=[C:7]([C:11]#[N:12])[CH:6]=1)[O:4][CH3:15]

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 595703134-(2,2,2-Trifluoro-1-hydroxyethyl)pyridine-2-carbonitrile

生成物 1

HCID 595703734-(2,2,2-Trifluoro-1-methoxyethyl)pyridine-2-carbonitrile収率 46.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To 4 ml of dimethylformamide were added 0.4 g of 4-(2,2,2-trifluoro-1-hydroxyethyl)pyridine-2-carbonitrile, 0.33 g of potassium carbonate and 0.34 g of methyl iodide, and the mixture was stirred at room temperature for 20 hours. Thereafter, an aqueous saturated ammonium chloride solution was added to the reaction solution, the resultant solution was extracted with ethyl acetate three times, the organic layers were combined, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.2 g of 4-(2,2,2-trifluoro-1-methoxyethyl)pyridine-2-carbonitrile.

後処理

  1. extractionthe resultant solution was extracted with ethyl acetate three times
  2. dry with materialdried with anhydrous magnesium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-388a4c6435284c00bd9126b5c2a66ade
出典データセット
uspto-grants-2012_11
特許番号
US08318776B2

反応ノート

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