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Sodium Cyanide → 5-Methyl-2-phenyl-2H-1,2,3-triazole-4-acetonitrile

HRID 478335
ノート
印刷プレビュー

反応式

HRID 478335 の反応式
[C-:1]#[N:2].[Na+].Cl[CH2:5][C:6]1[C:10]([CH3:11])=[N:9][N:8]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:7]=1.[OH-].[Na+]>CN(C=O)C>[CH3:11][C:10]1[C:6]([CH2:5][C:1]#[N:2])=[N:7][N:8]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8929Sodium CyanideHCID 14798Sodium HydroxideHCID 338434HCID 338434、化合物

生成物 1

HCID 5632655-Methyl-2-phenyl-2H-1,2,3-triazole-4-acetonitrile収率 90.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.8 g of sodium cyanide was suspended in 30 ml of DMF, and 5.0 g of 4-chloromethyl-5-methyl-2-phenyl-1,2,3-triazol was added under cooling with ice. After stirring for 3 hours at room temperature, an aqueous solution of sodium hydroxide was added to the reaction solution to make it alkaline, and extracted with toluene. The organic phase was washed with water and a saturated salt solution, then dried over anhydrous sodium sulfate. After the solvent was distilled off, the deposited crystals were washed with hexane to obtain 4.3 g of the aimed compound.

後処理

  1. temperatureunder cooling with ice
  2. extractionextracted with toluene
  3. washThe organic phase was washed with water
  4. dry with materiala saturated salt solution, then dried over anhydrous sodium sulfate
  5. distillationAfter the solvent was distilled off
  6. washthe deposited crystals were washed with hexane

出典と根拠

ORDレコード
ord-7991a7dcb39a4bcfb2dd08149983ef8e
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06642234B1

反応ノート

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