Nitric Acid → 4-Methoxy-1-nitrodibenzo[b,d]thiophene

HRID 15241노트

반응식

HRID 15241 반응식
[CH3:1][O:2][C:3]1[C:8]2[S:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[C:7]=2[CH:6]=[CH:5][CH:4]=1.[N+:16]([O-])([OH:18])=[O:17].O>C(O)(=O)C>[CH3:1][O:2][C:3]1[C:8]2[S:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[C:7]=2[C:6]([N+:16]([O-:18])=[O:17])=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 962WaterHCID 4583544-Methoxydibenzothiophene

생성물 1

HCID 122571114-Methoxy-1-nitrodibenzo[b,d]thiophene

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

4-Methoxy-dibenzothiophene (ii)(4.3 g, 20.0 mmol) was dissolved in glacial acetic acid (60 ml) and to this solution was added fuming nitric acid (3.37 ml) in a dropwise fashion ensuring that the temperature of the mixture did not rise above 25° C. The yellow suspension was stirred for a further 45 minutes before being poured carefully into water (200 ml) and stirred for 15 minutes. The yellow solid was removed by filtration and washed thoroughly with copious amounts of water and then hexanes. The residue thus obtained was then dried in a vacuum oven to give the title compound as a yellow solid which was used without any further purification. (5.19 g, 97%) m/z (LC-MS, ESP), RT=4.15 min, (M+H)=260.1

후처리

  1. customdid not rise above 25° C
  2. stirringstirred for 15 minutes
  3. customThe yellow solid was removed by filtration
  4. washwashed thoroughly with copious amounts of water
  5. customThe residue thus obtained
  6. customwas then dried in a vacuum oven

출처 및 근거

ORD 기록
ord-62273550bcdf4ce882d21ce51dc6e966
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732483B2

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