2-Bromo-4-trifluoromethylaniline → 4-Amino-3-cyanobenzotrifluoride

HRID 711689

反応式

HRID 711689 の反応式
Br[C:2]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[CH:5][C:3]=1[NH2:4].[Cu](C#N)[C:14]#[N:15]>CN1CCCC1=O.C(OCC)(=O)C>[NH2:4][C:3]1[CH:5]=[CH:6][C:7]([C:9]([F:12])([F:11])[F:10])=[CH:8][C:2]=1[C:14]#[N:15]

参加物

5

反応物 2

HCID 938992-Bromo-4-trifluoromethylanilineHCID 178418260HCID 178418260、化合物

生成物 1

HCID 126273614-Amino-3-cyanobenzotrifluoride

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

In a 20 mL microwave vial, 2-bromo-4-(trifluoromethyl)aniline (238 mg, 1 mmol) and copper cyanide (90 mg, 1 mmol) were dissolved in N-methylpyrrolidone (NMP) (10 mL). The reaction was placed in a microwave reactor for 5 minutes at 200° C. The crude was dissolved in ethyl acetate and the precipitate was removed by filtration. The clear solution was washed with water. The organic layer was collected, dried over sodium sulfate, and evaporated under vacuum. The residue was purified by Varia HPLC (10% acetonitrile/water) to give the title compound.

後処理

  1. customthe precipitate was removed by filtration
  2. washThe clear solution was washed with water
  3. customThe organic layer was collected
  4. dry with materialdried over sodium sulfate
  5. customevaporated under vacuum
  6. customThe residue was purified by Varia HPLC (10% acetonitrile/water)

出典と根拠

ORDレコード
ord-9801ae079fad4f028e95c62fb9d6110c
出典データセット
uspto-grants-2015_11
特許番号
US09181276B2

関連ノート

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