Nitric Acid → Stattic

HRID 554246노트

반응식

HRID 554246 반응식
[N+:1]([O-:4])(O)=[O:2].[S:5]1(=[O:15])(=[O:14])[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[CH:7]=[CH:6]1>S(=O)(=O)(O)O>[N+:1]([C:11]1[CH:12]=[CH:13][C:8]2[CH:7]=[CH:6][S:5](=[O:15])(=[O:14])[C:9]=2[CH:10]=1)([O-:4])=[O:2]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 69997Benzothiophene 1,1-dioxide

생성물 1

HCID 2779853Stattic수율 84%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

Nitric acid (10 mL) was slowly added to sulfuric acid (10 mL) at 0° C., and the mixture was stirred at the same temperature for 10 min. To this solution was slowly added 1-benzothiophene 1,1-dioxide (3.99 g) at 0° C., and the mixture was further stirred at the same temperature for 30 min. The reaction mixture was poured into ice water, and the mixture was extracted with ethyl acetate. The extract was washed twice with water, saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to give the title compound as a pale-yellow solid (yield 4.26 g, 84%).

후처리

  1. customat 0° C.
  2. stirringthe mixture was further stirred at the same temperature for 30 min
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed twice with water, saturated aqueous sodium hydrogencarbonate solution and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-e4f3bb9c71194648a0196fccda63007a
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08048909B2

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