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

HRID 1757493

반응식

HRID 1757493 반응식
[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

참가 물질

5

반응물 2

HCID 810862-MethoxybenzonitrileHCID 4984872Tributyltin azide

생성물 1

HCID 8589085-(2-Methoxyphenyl)-1H-tetrazole수율 98.1%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 7237O-Xylene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4592e26b89c444cbade63ed2b263f723
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05446121

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