Acetic Acid → 2,2-dimethyl-5,6-dinitro-1,3-benzodioxole

HRID 2248107ノート

反応式

HRID 2248107 の反応式
[N+:1]([O-:4])([OH:3])=O.C(O)(=O)C.[CH3:9][C:10]1([CH3:22])[O:14][C:13]2[CH:15]=[CH:16][C:17]([N+:19]([O-:21])=[O:20])=[CH:18][C:12]=2[O:11]1>O>[CH3:9][C:10]1([CH3:22])[O:11][C:12]2[CH:18]=[C:17]([N+:19]([O-:21])=[O:20])[C:16]([N+:1]([O-:4])=[O:3])=[CH:15][C:13]=2[O:14]1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 944Nitric AcidHCID 2330662,2-Dimethyl-5-nitro-1,3-benzodioxole

生成物 1

HCID 50472752,2-dimethyl-5,6-dinitro-1,3-benzodioxole収率 82%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 90% (fuming) nitric acid (22 ml) and glacial acetic acid (11 ml) cooled at 12° C. was treated in portions with solid compound from Example 3B (5.4 g, 27.7 mmoles) so as to maintain the temperature of <17° C. After the addition, stirring was continued for 15 minutes, when the internal temperature began to fall. The mixture was diluted to 100 ml with water, the yellow solid filtered, washed with water, taken up in CH2Cl2, dried (Na2SO4) and evaporated to give 5.43 g (82%) of pure title compound.

後処理

  1. temperatureto maintain the temperature of <17° C
  2. additionAfter the addition
  3. filtrationthe yellow solid filtered
  4. washwashed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated

出典と根拠

ORDレコード
ord-a29cdd118e834e90807861c774570d23
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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