Acetonitrile → 4-Amino-2,5,6-trifluorobenzene-1,3-dicarbonitrile

HRID 65450노트

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HRID 65450 반응식
[F:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([F:10])[C:5]([C:11]#[N:12])=[C:4](F)[C:3]=1[F:14].C(=O)(O)[O-].[Na+].C(#[N:22])C>N>[NH2:22][C:4]1[C:3]([F:14])=[C:2]([F:1])[C:7]([C:8]#[N:9])=[C:6]([F:10])[C:5]=1[C:11]#[N:12]

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 516892Sodium BicarbonateHCID 608182Tetrafluoroisophthalonitrile

생성물 1

HCID 135404564-Amino-2,5,6-trifluorobenzene-1,3-dicarbonitrile수율 61%

시약·촉매·용매 1

HCID 222Ammonia용매

실험 절차

To a solution of 2.0 g of tetrafluoroisophthalonitrile in 20 ml of acetonitrile, 0.6 ml of 28% aqueous ammonia was dropwise added. After the dropwise addition, the mixture was stirred at room temperature for one hour. An aqueous sodium bicarbonate solution was added to the mixture and the resultant mixture was extracted with chloroform and was washed with an aqueous sodium chloride solution. After drying with sodium sulfate, the chloroform was distilled off to obtain yellow crystal. The resultant crystal was recrystallized from chloroform to obtain 1.2 g (61% yield) of the desired compound No. 1.

후처리

  1. additionAfter the dropwise addition
  2. extractionthe resultant mixture was extracted with chloroform
  3. washwas washed with an aqueous sodium chloride solution
  4. dry with materialAfter drying with sodium sulfate
  5. distillationthe chloroform was distilled off
  6. customto obtain yellow crystal
  7. customThe resultant crystal was recrystallized from chloroform

출처 및 근거

ORD 기록
ord-a6445229094340d9a835bd8167833b6b
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614742

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