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Water → 5-Fluoro-8-nitro-3,4-dihydronaphthalen-1(2H)-one

HRID 2257838
ノート
印刷プレビュー

反応式

HRID 2257838 の反応式
[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][C:7]2=[O:12].[N+:13]([O-])([O-:15])=[O:14].[K+].O>S(=O)(=O)(O)O>[F:1][C:2]1[CH:11]=[CH:10][C:9]([N+:13]([O-:15])=[O:14])=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][C:7]2=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 24434Potassium NitrateHCID 154910385-Fluoro-1,2,3,4-tetrahydronaphthalen-1-one

生成物 1

HCID 224494055-Fluoro-8-nitro-3,4-dihydronaphthalen-1(2H)-one

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

実験手順

14 gm of the compound prepared in (7) above was dissolved into 100 ml of concentrated sulfuric acid. After cooling the solution, a solution of 9.05 gm of potassium nitrate in 80 ml of concentrated sulfuric acid was added dropwise while maintaining the internal temperature below 5° C. The stirring was continued for a further 30 minutes. The resultant reaction mixture was poured into ice-cooled water and extracted with chloroform. The extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated and residue was recrystallized in methanol to obtain 9.15 gm of the title compound.

後処理

  1. temperatureAfter cooling the solution
  2. temperaturewhile maintaining the internal temperature below 5° C
  3. customThe resultant reaction mixture
  4. additionwas poured into ice-
  5. extractionextracted with chloroform
  6. washThe extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe solvent was evaporated
  9. customresidue was recrystallized in methanol

出典と根拠

ORDレコード
ord-0b258327cc8446cab014a74315cff3cc
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05658920

反応ノート

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