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

HRID 478335
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HRID 478335 반응식
[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
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참가 물질

5

반응물 3

HCID 8929Sodium CyanideHCID 14798Sodium HydroxideHCID 338434HCID 338434, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7991a7dcb39a4bcfb2dd08149983ef8e
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06642234B1

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