Methyl iodide → HCID 67187925, 화합물

HRID 868841노트

반응식

HRID 868841 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 67187925HCID 67187925, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

(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.

후처리

  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

출처 및 근거

ORD 기록
ord-cdd4ee6bdc2e43699447f90c028d08f6
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969348B2

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