Water → HCID 18357786、化合物

HRID 427991ノート

反応式

HRID 427991 の反応式
[CH3:1][C:2]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][C:13]#[N:14].[H-].[Na+].[CH2:22](I)[CH3:23].O>CN(C)C=O>[CH3:1][C:2]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH:12]([CH2:22][CH3:23])[C:13]#[N:14]

参加物

6

反応物 4

HCID 962WaterHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 11118528HCID 11118528、化合物

生成物 1

HCID 18357786HCID 18357786、化合物収率 86%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-[2-(2,5-dimethylphenoxymethyl)phenyl]acetonitrile (2.00 g, 8.0 mmol) in N,N-dimethylformamide (20 ml) was stirred at 0° C. 60% oily sodium hydride (0.38 g, 9.5 mmol) was added thereto, and then ethyl iodide (1.37 g, 8.8 mmol) was added dropwise over 5 minutes. After 1 hour, water was added, and the mixture was extracted with ethyl acetate, washed successively with water and saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=19/1) to give the desired compound 2-[2-(2,5-dimethylphenoxymethyl)phenyl]butyronitrile (1.91 g, 86%) as an oil.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed successively with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated
  5. customthe residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=19/1)

出典と根拠

ORDレコード
ord-39bcea21a3454ab79de60da95db07310
出典データセット
uspto-grants-2001_11
特許番号
US06313150B1

反応ノート

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