Acetic Acid → 2,2-Dimethyl-5-nitro-1,3-benzodioxole

HRID 2248106ノート

反応式

HRID 2248106 の反応式
[N+:1]([O-:4])(O)=[O:2].C(O)(=O)C.[CH3:9][C:10]1([CH3:19])[O:14][C:13]2[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=2[O:11]1>O>[CH3:9][C:10]1([CH3:19])[O:11][C:12]2[CH:18]=[CH:17][C:16]([N+:1]([O-:4])=[O:2])=[CH:15][C:13]=2[O:14]1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 944Nitric AcidHCID 2858692,2-dimethyl-2H-1,3-benzodioxole

生成物 1

HCID 2330662,2-Dimethyl-5-nitro-1,3-benzodioxole

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 70% (conc.) nitric acid (20 ml) and glacial acetic acid (10 ml) cooled at 12° C. was treated by drops with 5 g (33.3 mmole) of the compound of Example 3A at a rate to maintain the temperature at 15°-20° C. Stirring was continued for 15 minutes after addition, then the brown slurry was diluted to 100 ml with water and filtered. The solid was washed with water, taken up in CH2Cl2, dried (Na2SO4) and evaporated to 5.40 g (83%) of pure yellow mononitro title compound.

後処理

  1. temperatureto maintain the temperature at 15°-20° C
  2. additionafter addition
  3. filtrationfiltered
  4. washThe solid was washed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated to 5.40 g (83%) of pure yellow mononitro title compound

出典と根拠

ORDレコード
ord-59ccbc6a7b29438d8b15da99e1c42378
出典データセット
uspto-grants-1991_08
特許番号
US05037983

反応ノート

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