Methyl iodide → HCID 178482153、化合物

HRID 499801ノート

反応式

HRID 499801 の反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]2=S)=[CH:4][CH:3]=1.CI.[CH3:17][NH2:18]>CC#N.CO>[I:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:13]=[CH:12][CH:11]=[CH:10]/[C:9]/2=[N:18]\[CH3:17])=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 6329MethylamineHCID 86616333HCID 86616333、化合物

生成物 1

HCID 178482153HCID 178482153、化合物収率 61.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6342Acetonitrile溶媒

実験手順

To a solution of 1-(4-iodophenyl)pyridine-2(1H)-thione (98 mg, 0.31 mmol) in CH3CN (5 mL), CH3I (0.25 mL, 4.0 mmol) was added. After being stirred at room temperature overnight, the mixture was concentrated in vacuo to give a solid. The solid was dissolved in MeOH (7 mL). To the solution, CH3NH2 (2M in THF, 0.80 mL, 1.6 mmol) was added. After being stirred at room temperature overnight, the mixture was purified by HPLC to give (E)-N-(1-(4-iodophenyl)pyridin-2(1H)-ylidene)methanamine (59 mg).

後処理

  1. concentrationthe mixture was concentrated in vacuo
  2. customto give a solid
  3. stirringAfter being stirred at room temperature overnight
  4. customthe mixture was purified by HPLC

出典と根拠

ORDレコード
ord-369a253d00d24287a9ea46c8c4f63139
出典データセット
uspto-grants-2010_08
特許番号
US07767697B2

反応ノート

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