Methyl iodide → HCID 20285784, compound

HRID 263129Notes

Reaction equation

HRID 263129 reaction equation
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[N:11]=[C:10]([C:12]3[CH:17]=[CH:16][N:15]=[CH:14][N:13]=3)[NH:9][N:8]=2)=[N:3][CH:2]=1.[H-].[CH3:19]I>O1CCCC1>[CH3:19][N:8]1[C:7]([C:4]2[CH:5]=[CH:6][N:1]=[CH:2][N:3]=2)=[N:11][C:10]([C:12]2[CH:17]=[CH:16][N:15]=[CH:14][N:13]=2)=[N:9]1

Participants

5

Procedure

To 3,5-bis(4-pyrimidinyl)-1,2,4-triazole (2.3 g.) in dry tetrahydrofuran (125 ml.) is added 57% sodimm hydride in mineral oil (0.46 g.). After refluxing 0.5 hour, methyl iodide (1.4 g.) is added and the mixture is heated at reflux an additional three hours. The reaction mixture is cooled, filtered and concentrated to a solid which after recrystallization yields substantially pure 1-methyl-3,5-bis(4-pyrimidinyl)-1,2,4-triazole.

Workup

  1. temperatureAfter refluxing 0.5 hour
  2. temperaturethe mixture is heated
  3. temperatureat reflux an additional three hours
  4. temperatureThe reaction mixture is cooled
  5. filtrationfiltered
  6. concentrationconcentrated to a solid which
  7. customafter recrystallization

Sources & evidence

ORD record
ord-4276e447be0d47838aa28fc9af6ece7a
Source dataset
uspto-grants-1979_05
Patent number
US04156085

Reaction notes

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