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

HRID 471552

반응식

HRID 471552 반응식
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]

참가 물질

5

반응물 2

HCID 938992-Bromo-4-trifluoromethylanilineHCID 178418260HCID 178418260, 화합물

생성물 1

HCID 126273614-Amino-3-cyanobenzotrifluoride

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-0839b86277dd4bccb177a00036985fcc
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633186B2

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