Methyl iodide → HCID 67187925、化合物

HRID 868841ノート

反応式

HRID 868841 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4]([CH2:11][C:12]#[N:13])=[CH:5][NH:6]2.[H-].[Na+].[CH3:16]I>C1COCC1>[CH3:16][N:6]1[C:7]2[C:3](=[C:2]([CH3:1])[CH:10]=[CH:9][CH:8]=2)[C:4]([CH2:11][C:12]#[N:13])=[CH:5]1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 24905095(4-Methyl-1H-indol-3-yl)acetonitrile

生成物 1

HCID 67187925HCID 67187925、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

(4-Methyl-1H-indol-3-yl)-acetonitrile (540 mg, 3.2 mmol), is taken up in dry THF (10.3 mL), cooled to zero, and sodium hydride (228 mg, 60% in mineral oil, 6 mmol) is added to the stirring solution. The reaction is stirred for 15 minutes at zero and methyl iodide (0.26 mL, 4 mmol) is added. The solution is stirred for 20 minutes at zero, and quenched by the slow addition of saturated aqueous ammonium chloride. The compound is extracted with ethyl acetate, dried (Na2SO4), filtered, and evaporated in vacuo to give a solid that is purified on silica gel with hexanes/ethylacetate as the eluent (1.0 g, 5 mmol, 71%) LC/MS (M++1): 185.5.

後処理

  1. additionis added to the stirring solution
  2. additionis added
  3. customquenched by the slow addition of saturated aqueous ammonium chloride
  4. extractionThe compound is extracted with ethyl acetate
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. customto give a solid

出典と根拠

ORDレコード
ord-cdd4ee6bdc2e43699447f90c028d08f6
出典データセット
uspto-grants-2015_03
特許番号
US08969348B2

反応ノート

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