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Dibenzofuran → 3-Nitrodibenzofuran

HRID 1022352
ノート
印刷プレビュー

反応式

HRID 1022352 の反応式
[CH:1]1[C:9]2[C:8]3[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=3[O:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[N+:14]([O-])([OH:16])=[O:15]>FC(F)(F)C(O)=O>[N+:14]([C:3]1[CH:2]=[CH:1][C:9]2[C:8]3[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=3[O:6][C:5]=2[CH:4]=1)([O-:16])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 568DibenzofuranHCID 944Nitric Acid

生成物 1

HCID 728973-Nitrodibenzofuran収率 80.4%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒2 回

実験手順

To 80 mL trifluoroacetic acid in a 250 mL round bottom flask was added dibenzofuran (7.06 g, 42 mmol) and stirred vigorously to dissolve the content at room temperature. The solution was then cooled on ice and 1.2 equivalent 70% HNO3 (4.54 g, 50.40 mmol) in 20 mL trifluoroacetic acid was poured into the stirred solution slowly. After stirring for 30 minutes contents from the flask was poured into 150 mL ice-water and stirred for another 15 minutes. Off white color precipitate was then filtered out and finally washed with 2M NaOH and water. Moist material was then recrystallized from 1.5 L boiling ethanol in the form of light yellow color crystal. 7.2 g of product was isolated.

後処理

  1. dissolutionto dissolve the content at room temperature
  2. additionwas poured into the stirred solution slowly
  3. stirringAfter stirring for 30 minutes contents from the flask
  4. stirringstirred for another 15 minutes
  5. filtrationOff white color precipitate was then filtered out
  6. washfinally washed with 2M NaOH and water
  7. customMoist material was then recrystallized from 1.5 L

出典と根拠

ORDレコード
ord-df632192c9124985bb71e8f817205bc7
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722205B2

反応ノート

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