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

HRID 129562

反応式

HRID 129562 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 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).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  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-24f3d94f5f7e4bb690354a44a4f20d20
出典データセット
uspto-grants-1995_11
特許番号
US05468867

関連ノート

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