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

HRID 2165306

反応式

HRID 2165306 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-68cc3041ca384c2fa151e44426e84d21
出典データセット
uspto-grants-1990_07
特許番号
US04939265

関連ノート

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