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

HRID 1893561

反応式

HRID 1893561 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 45504615-Methyl-6-nitro-1,3-benzodioxole収率 90%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d622537d0d57496f8d10b97bbaadf49d
出典データセット
uspto-grants-2013_08
特許番号
US08513235B2

関連ノート

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