1-Indanone → 6-Nitroindan-1-one

HRID 324984

反応式

HRID 324984 の反応式
[C:1]1(=[O:10])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][CH2:2]1.[N+:11]([O-])([O-:13])=[O:12].[K+]>S(=O)(=O)(O)O>[N+:11]([C:7]1[CH:8]=[C:9]2[C:4]([CH2:3][CH2:2][C:1]2=[O:10])=[CH:5][CH:6]=1)([O-:13])=[O:12]

参加物

4

反応物 2

HCID 67351-IndanoneHCID 24434Potassium Nitrate

生成物 1

HCID 905626-Nitroindan-1-one収率 129.5%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of 1-indanone (25.0 g, 189 mmol) in concentrated sulfuric acid (84 mL) at 0° C. was added a solution of potassium nitrate (8.33 g, 82.4 mmol) in sulfuric acid (40 mL) at a rate sufficient to maintain an internal temperature below 15° C. After the addition was complete, the reaction was allowed to stir at 0° C. for 1 hour. The reaction mixture was then poured into crushed ice and stirred vigorously for 30 minutes. The suspension was then filtered, air dried, and purified by liquid chromatography (50 ethyl acetate/toluene) to provide 18.90 g of the title compound. (56%).

後処理

  1. temperatureto maintain an internal temperature below 15° C
  2. additionAfter the addition
  3. additionThe reaction mixture was then poured
  4. custominto crushed ice
  5. stirringstirred vigorously for 30 minutes
  6. filtrationThe suspension was then filtered
  7. customair dried
  8. custompurified by liquid chromatography (50 ethyl acetate/toluene)

出典と根拠

ORDレコード
ord-ed7ce624495248b9883aa0ef01b11b0c
出典データセット
uspto-grants-2001_04
特許番号
US06221876B1

関連ノート

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