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

HRID 979052

반응식

HRID 979052 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-02e5eba2d86747a6ad61fc9c271d97c8
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04666908

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