2-Methoxybenzonitrile → 5-(2-Methoxyphenyl)-1H-tetrazole

HRID 1757493ノート

反応式

HRID 1757493 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[O:9][CH3:10])#[N:2].C([Sn]([N:24]=[N+:25]=[N-:26])(CCCC)CCCC)CCC>C1(C)C(C)=CC=CC=1.C(OCC)C>[CH3:10][O:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:1]1[N:24]=[N:25][NH:26][N:2]=1

参加物

5

反応物 2

HCID 810862-MethoxybenzonitrileHCID 4984872Tributyltin azide

生成物 1

HCID 8589085-(2-Methoxyphenyl)-1H-tetrazole収率 98.1%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 7237O-Xylene溶媒

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 5hours. 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).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 5hours
  3. temperatureThe reaction mixture then was cooled
  4. customAnhydrous hydrochloric acid was bubbled into the mixture
  5. customa white precipitate formed
  6. filtrationThe precipitate was collected by suction filtration
  7. washwashed repeatedly with diethyl ether
  8. customDrying

出典と根拠

ORDレコード
ord-4592e26b89c444cbade63ed2b263f723
出典データセット
uspto-grants-1995_08
特許番号
US05446121

反応ノート

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