p-Toluenesulfonic acid → 1,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethene

HRID 1199219ノート

反応式

HRID 1199219 の反応式
[F: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[F:25])(O)[CH2:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.C(OCC)C>[F: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[F:1])=[CH:10][C:11]1[N:15]([CH3:16])[N:14]=[N:13][N:12]=1

参加物

5

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 147239921,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol

生成物 1

HCID 147239931,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethene

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

実験手順

A suspension of 1,1-bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol (7.3 g, 21.0 mmoles) in toluene (200 mL) with p-toluene sulfonic acid (3 g) and the mixture heated at reflux for 14 hours. After cooling, the mixture was diluted with diethyl ether and extracted with saturated sodium bicarbonate solution and water. The organic layer was dried (MgSO4) and evaporated. The residue was triturated with isopropyl ether to give the title compound; m.p.=58°-60° C.

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 14 hours
  3. temperatureAfter cooling
  4. extractionextracted with saturated sodium bicarbonate solution and water
  5. dry with materialThe organic layer was dried (MgSO4)
  6. customevaporated
  7. customThe residue was triturated with isopropyl ether

出典と根拠

ORDレコード
ord-12d2a476afd14a10a7e6bc9c105811b5
出典データセット
uspto-grants-1990_02
特許番号
US04898949

反応ノート

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