Methyl iodide → HCID 70982521、化合物

HRID 922597ノート

反応式

HRID 922597 の反応式
[I:1][C:2]1[N:3]=[CH:4][N:5]([CH2:8][C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)[C:6]=1[I:7].I[CH3:20]>C(#N)C>[I-:1].[I:7][C:6]1[N:5]([CH2:8][C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)[CH2:4][NH+:3]([CH3:20])[C:2]=1[I:1]

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 70982117HCID 70982117、化合物

生成物 1

HCID 70982521HCID 70982521、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4,5-diiodoimidazole (5.0 mmol) and KOH (5.0 mmol) were placed in a round bottom flask with 50 mL THF. The mixture was brought to reflux and stirred 0.5 h until KOH was consumed. 2-bromomethylnapthalene (5.0 mmol) was added and the solution was stirred at reflux for 17 hours. KBr was removed by vacuum filtration and the filtrate was collected. The volatiles were removed by rotary evaporation to give 4,5-diiodo-1-(naphthalen-2-ylmethyl)-1H-imidazole as a off white solid. 4,5-diiodo-1-(naphthalen-2-ylmethyl)-1H-imidazole was dissolved in acetonitrile in a round bottom flask. The solution was brought to reflux and excess iodomethane was added. The reaction was stirred at reflux for overnight after which time it was cooled. The resulting yellow precipitate was collected by filtration and analyzed. 1H NMR (300 MHz, d6-DMSO): δ 3.88 (s), 5.64 (s), 7.47-7.60 (m), 7.89-8.02 (m), 9.57 (s) ppm.

後処理

  1. temperatureto reflux
  2. temperatureat reflux for overnight after which time it
  3. temperaturewas cooled
  4. filtrationThe resulting yellow precipitate was collected by filtration

出典と根拠

ORDレコード
ord-da2c8d6ec44c45d19ca9751c0aa369cf
出典データセット
uspto-grants-2016_03
特許番号
US09278951B2

反応ノート

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