p-Toluenesulfonic acid → 2,3-Dihydro-7-nitro-1-benzoxepin

HRID 1613611ノート

反応式

HRID 1613611 の反応式
O[CH:2]1[C:8]2[CH:9]=[C:10]([N+:13]([O-:15])=[O:14])[CH:11]=[CH:12][C:7]=2[O:6][CH2:5][CH2:4][CH2:3]1.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[N+:13]([C:10]1[CH:11]=[CH:12][C:7]2[O:6][CH2:5][CH2:4][CH:3]=[CH:2][C:8]=2[CH:9]=1)([O-:15])=[O:14]

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 14580514HCID 14580514、化合物

生成物 1

HCID 145805152,3-Dihydro-7-nitro-1-benzoxepin

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

300 ml of toluene are poured over 25.1 g (0.12 mole) of 5-hydroxy-7-nitro-2,3,4,5-tetrahydro-1-benzoxepin and, with the addition of 1.5 g of p-toluenesulfonic acid, the mixture is refluxed with a water trap for 2 hours. The cold reaction solution is washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution, dried over sodium sulfate and filtered, and the solvent is evaporated off in vacuo. The residue is a solid of melting point 94°-95.5° C.

後処理

  1. temperaturethe mixture is refluxed with a water trap for 2 hours
  2. washThe cold reaction solution is washed with saturated sodium bicarbonate solution, water and saturated sodium chloride solution
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customthe solvent is evaporated off in vacuo

出典と根拠

ORDレコード
ord-8d8a62111e8b48b684dea9c1090f4c05
出典データセット
uspto-grants-1993_03
特許番号
US05194442

反応ノート

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