Potassium Iodide → 1,3-dimethyl-4-nitro-1H-pyrazole-5-carbonitrile

HRID 979052

反応式

HRID 979052 の反応式
[CH3:1][N:2]1[C:6](Cl)=[C:5]([N+:8]([O-:10])=[O:9])[C:4]([CH3:11])=[N:3]1.[C-]#N.[K+].[I-].[K+].[CH3:17][N:18](C=O)C>C(#N)C>[CH3:1][N:2]1[C:6]([C:17]#[N:18])=[C:5]([N+:8]([O-:10])=[O:9])[C:4]([CH3:11])=[N:3]1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 9032Potassium CyanideHCID 2795155-Chloro-1,3-dimethyl-4-nitro-1H-pyrazole

生成物 1

HCID 965071,3-dimethyl-4-nitro-1H-pyrazole-5-carbonitrile

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Fifty-five g of 1,3-dimethyl-4-nitro-5-chloropyrazole was dissolved in 400 ml acetonitrile and 17.45 g potassium cyanide added, followed by 0.5 g potassium iodide and 5 ml DMF. The mixture was refluxed for 22 hours, then cooled, and filtered. The filtrate was concentrated under reduced pressure, then added to stirred water. The resulting percipitate was collected, dried, and recyrstallized in isopropanol. mp, 85°-87° C. A second recrystallization again in ethanol gave the product having increased purity, mp 96°-98° C.

後処理

  1. temperatureThe mixture was refluxed for 22 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. additionadded
  6. customThe resulting percipitate was collected
  7. customdried
  8. custommp, 85°-87° C
  9. customA second recrystallization again in ethanol
  10. customgave the product
  11. temperaturehaving increased purity, mp 96°-98° C.

出典と根拠

ORDレコード
ord-02e5eba2d86747a6ad61fc9c271d97c8
出典データセット
uspto-grants-1987_05
特許番号
US04666908

関連ノート

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