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

HRID 36031

반응식

HRID 36031 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 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).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 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

출처 및 근거

ORD 기록
ord-bebdd46407ed4d14828dd44daa521bd6
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05412102

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