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

HRID 65450ノート

反応式

HRID 65450 の反応式
[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]

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 516892Sodium BicarbonateHCID 608182Tetrafluoroisophthalonitrile

生成物 1

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

試薬・触媒・溶媒 1

HCID 222Ammonia溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a6445229094340d9a835bd8167833b6b
出典データセット
uspto-grants-1986_09
特許番号
US04614742

反応ノート

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