Potassium bisulfate → 1,1-Bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethene

HRID 1199205

반응식

HRID 1199205 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]([C:18]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:19]=1[CH3:25])(O)[CH2:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1.S([O-])(O)(=O)=O.[K+]>C(Cl)Cl>[CH3:25][C:19]1[CH:20]=[C:21]([CH3:24])[CH:22]=[CH:23][C:18]=1[C:9]([C:3]1[CH:4]=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=1[CH3:1])=[CH:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1

참가 물질

4

반응물 2

HCID 516920Potassium bisulfateHCID 147239461,1-Bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol

생성물 1

HCID 147239471,1-Bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethene수율 69.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 1,1-bis(2,4-dimethylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol (1.8 g, 5.4 mmoles) and potassium hydrogen sulfate (100 mg) in a 50 ml flask was placed in an oil bath preheated to 190° C. After 15 minutes, the melt was cooled and methylene chloride added to the residue. The insolubles were removed and the solution evaporated. The residue was crystallized from isopropyl ether to give 1.2 g of the title compound; m.p.=143°-143.5° C.

후처리

  1. customwas placed in an oil bath
  2. custompreheated to 190° C
  3. temperaturethe melt was cooled
  4. customThe insolubles were removed
  5. customthe solution evaporated
  6. customThe residue was crystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-ce97a7ace556495ca11fa365914a708d
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898949

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