反応 #216744

ord-24f3d94f5f7e4bb690354a44a4f20d20

反応方程式

COc1ccccc1C#N
1-cyano-2-methoxybenzene
CCC[CH2][Sn]([CH2]CCC)([CH2]CCC)[N]=[N+]=[N-]
tributyltin azide
COc1ccccc1-c1nn[nH]n1
5-(2-methoxyphenyl)-2H-tetrazole
収率 98.1%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度under reflux for 5 hours
  3. 3
    温度The reaction mixture then was cooled
  4. 4
    その他Anhydrous hydrochloric acid was bubbled into the mixture
  5. 5
    その他a white precipitate formed
  6. 6
    ろ過The precipitate was collected by suction filtration
  7. 7
    洗浄washed repeatedly with diethyl ether
  8. 8
    その他Drying

実験手順

A mixture of 1-cyano-2-methoxybenzene (1.02 g, 7.7 mmol) and tributyltin azide (3.4 g, 10.0 mmol) in 3.0 mL of xylene was heated under reflux for 5 hours. The reaction mixture then was cooled and diluted with diethyl ether. Anhydrous hydrochloric acid was bubbled into the mixture and a white precipitate formed. The precipitate was collected by suction filtration and washed repeatedly with diethyl ether. Drying gave 5-(2-methoxyphenyl)-2H-tetrazole (1.33 g, 7.55 mmol).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05468867uspto-grants-1995_11