Potassium Nitrate → 5-Bromo-4-chloro-3-nitroisatoic anhydride

HRID 1845069

反応式

HRID 1845069 の反応式
[Br:1][C:2]1[CH:13]=[C:6]2[C:7]([O:9][C:10](=[O:12])[NH:11][C:5]2=[CH:4][C:3]=1[Cl:14])=[O:8].[N+:15]([O-])([O-:17])=[O:16].[K+]>OS(O)(=O)=O>[Br:1][C:2]1[CH:13]=[C:6]2[C:7]([O:9][C:10](=[O:12])[NH:11][C:5]2=[C:4]([N+:15]([O-:17])=[O:16])[C:3]=1[Cl:14])=[O:8]

参加物

4

反応物 2

HCID 24434Potassium NitrateHCID 866083925-Bromo-4-chloroisatoic anhydride

生成物 1

HCID 866083935-Bromo-4-chloro-3-nitroisatoic anhydride収率 50%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

反応条件

温度
-20 °C

実験手順

5.4 g (20 mmol) of 5-bromo-4-chloroisatoic anhydride was suspended in 20 ml of conc. H2SO4 at −10° C. and cooled to −20° C. 2.1 g (21 mmol) of potassium nitrate was dissolved in 6 mL of sulfuric acid and cooled to 0° C., was then added dropwise to the reaction mixture. The reaction mixture was then stirred −10° C. for 15 min and warmed to room temperature overnight. The mixture was poured in to a beaker containing ice. The resulting solid was collected by filtration, washed with cold water and dried to produce 3.2 g (50%) of 5-bromo-4-chloro-3-nitroisatoic anhydride. LCMS: 323 (M+1)+.

後処理

  1. temperaturecooled to 0° C.
  2. additionwas then added dropwise to the reaction mixture
  3. temperaturewarmed to room temperature overnight
  4. additionThe mixture was poured in to a beaker
  5. additioncontaining ice
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with cold water
  8. customdried

出典と根拠

ORDレコード
ord-634087ee0c854aeca176c2d8e49f734b
出典データセット
uspto-grants-2015_02
特許番号
US08946259B2

関連ノート

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