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

HRID 1583785ノート

反応式

HRID 1583785 の反応式
[N+:1]([O-:4])(O)=[O:2].[CH3:5][C:6]1([CH3:15])[O:10][C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[O:7]1>C(O)(=O)C>[CH3:5][C:6]1([CH3:15])[O:7][C:8]2[CH:14]=[CH:13][C:12]([N+:1]([O-:4])=[O:2])=[CH:11][C:9]=2[O:10]1

参加物

4

反応物 2

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

生成物 1

HCID 2330662,2-Dimethyl-5-nitro-1,3-benzodioxole収率 33.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

24 ml of nitric acid (d=1.4) in 60 ml of glacial acetic acid were added dropwise at 15°-20° C. to 39.0 g of 2,2-dimethyl-1,3-benzodioxole in 200 ml of glacial acetic acid. After stirring at room temperature for 3 hours, the mixture was poured into ice/water and extracted twice with 1 l of methylene chloride. The organic phase was washed neutral with water, dried over sodium sulfate and evaporated in vacuo. The residue, recrystallized from methanol, gave 17.0 g (33.5% of theory) of 2,2-dimethyl-5-nitro-1,3-benzodioxole of melting point 88°-90° C.

後処理

  1. extractionextracted twice with 1 l of methylene chloride
  2. washThe organic phase was washed neutral with water
  3. dry with materialdried over sodium sulfate
  4. customevaporated in vacuo
  5. customThe residue, recrystallized from methanol

出典と根拠

ORDレコード
ord-af1361c8594d42afa483d961e2f19df9
出典データセット
uspto-grants-1985_11
特許番号
US04554280

反応ノート

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