Methyl iodide → HCID 178512035、化合物

HRID 499799ノート

反応式

HRID 499799 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.[N:17]#[C:18][NH2:19].O.NN>CC#N>[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:19]\[C:18]#[N:17])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 9864CyanamideHCID 24654Hydrazine hydrate (1:1)HCID 86616333HCID 86616333、化合物

生成物 1

HCID 178512035HCID 178512035、化合物収率 13.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

To a solution of 1-(4-iodophenyl)pyridine-2(1H)-thione (180 mg, 0.575 mmol) in CH3CN (15 mL), CH3I (0.50 mL, 8.0 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 CH3CN (5 mL). To the solution, cyanamide (200 mg, 4.76 mmol) and hydrazine monohydrate (0.100 mL, 2.06 mmol) were added. After being stirred at room temperature for 2 h, the mixture was purified by HPLC to give (E)-(1-(4-iodophenyl)pyridin-2(1H)-ylidene)cyanamide (25 mg).

後処理

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

出典と根拠

ORDレコード
ord-78e284f3339045caa9a014e899353d75
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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