Nitric Acid → 5-Methyl-6-nitro-1,3-benzodioxole

HRID 1893561

반응식

HRID 1893561 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]2[O:6][CH2:7][O:8][C:4]=2[CH:3]=1.[N+:11]([O-])([OH:13])=[O:12]>C(Cl)(Cl)Cl.ClCCl>[CH3:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:5]2[O:6][CH2:7][O:8][C:4]=2[CH:3]=1

참가 물질

5

반응물 2

HCID 944Nitric AcidHCID 815641,3-Benzodioxole, 5-methyl-

생성물 1

HCID 45504615-Methyl-6-nitro-1,3-benzodioxole수율 90%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

5-Methyl-1,3-benzodioxole (8.00 g, 58.8 mmol) was dissolved in chloroform (160 ml), and the mixture was stirred under ice-cooling. To this solution was gradually added 60% nitric acid (20 ml), and the mixture was stirred at room temperature for 30 min. The reaction mixture was diluted with dichloromethane, washed with water and saturated aqueous sodium hydrogen carbonate, and dried over potassium carbonate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give the title compound (9.58 g, yield 90%) as a pale-yellow solid.

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 30 min
  3. washwashed with water and saturated aqueous sodium hydrogen carbonate
  4. dry with materialdried over potassium carbonate
  5. filtrationThe insoluble material was filtered off
  6. concentrationthe solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d622537d0d57496f8d10b97bbaadf49d
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513235B2

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