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Potassium Iodide → (4-Iodophenylethynyl)trimethylsilane

HRID 2262329
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HRID 2262329 반응식
[CH3:1][Si:2]([C:5]#[C:6][C:7]1[CH:13]=[CH:12][C:10](N)=[CH:9][CH:8]=1)([CH3:4])[CH3:3].N([O-])=O.[Na+].[I-:18].[K+]>Cl>[CH3:1][Si:2]([C:5]#[C:6][C:7]1[CH:13]=[CH:12][C:10]([I:18])=[CH:9][CH:8]=1)([CH3:4])[CH3:3]
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참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 110524294-[(Trimethylsilyl)ethynyl]anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 11808725(4-Iodophenylethynyl)trimethylsilane수율 92%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

As shown in the following Reaction 2, 250 mg (1.32 mmol) of 4-trimethylsilylethynylaniline obtained in A of Example 1-1 was melted in 3 mL of hydrochloric acid at the temperature of 0° C., and 94 mg (1.37 mmol, 1.04 eq) of sodium nitrite was added thereto, and then the reaction solution was stirred for 1 hour. After completion of stirring, 280 mg (1.69 mmol, 1.28 eq) of potassium iodide was added to the reaction solution, and then the reaction solution was stirred at room temperature for 12 hours. Next, the reaction solution was extracted with ether 2 times and 1 time with 1M sodium chloride aqueous solutions 1 time. The organic solvent layer was dehydrated with magnesium sulfate, filtered, and then distilled under reduced pressure. The compound distilled under reduced pressure was purified with an alumina column chromatography (mobile phase: hexane) to obtain 360 mg of 4-trimethylsilylethynyl iodobenzene with the yield of 92%. NMR data of the obtained compound is as follows. [1H NMR (400 MHz, CDCl3): δ 0.23-0.27 (m, 9H), 7.16 (d, 2H), 7.69 (d, 2H)].

후처리

  1. customobtained in A of Example 1-1
  2. additionwas added
  3. stirringAfter completion of stirring
  4. stirringthe reaction solution was stirred at room temperature for 12 hours
  5. extractionNext, the reaction solution was extracted with ether 2 times and 1 time with 1M sodium chloride aqueous solutions 1 time
  6. filtrationfiltered
  7. distillationdistilled under reduced pressure
  8. distillationThe compound distilled under reduced pressure
  9. customwas purified with an alumina column chromatography (mobile phase: hexane)

출처 및 근거

ORD 기록
ord-3b967c2ef80a4622b227c53c6895959b
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07850872B2

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