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

HRID 1613611노트

반응식

HRID 1613611 반응식
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]

참가 물질

4

반응물 2

HCID 6101p-Toluenesulfonic acidHCID 14580514HCID 14580514, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d8a62111e8b48b684dea9c1090f4c05
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194442

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