Hydrochloric Acid → 4-Amino-5-fluoro-2-(trifluoromethyl)benzonitrile

HRID 1504945노트

반응식

HRID 1504945 반응식
[C:1]([C:3]1[C:8]([C:9]([F:12])([F:11])[F:10])=[CH:7][C:6]([NH:13]C(=O)C)=[C:5]([F:17])[CH:4]=1)#[N:2].Cl>CCO>[NH2:13][C:6]1[C:5]([F:17])=[CH:4][C:3]([C:1]#[N:2])=[C:8]([C:9]([F:12])([F:10])[F:11])[CH:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 68292028N-(4-cyano-2-fluoro-5-(trifluoromethyl)phenyl)acetamide

생성물 1

HCID 682929284-Amino-5-fluoro-2-(trifluoromethyl)benzonitrile수율 99.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of compound 24 (800 mg, 3.25 mmol) in EtOH (10 mL) was added concentrated HCl solution (12N, 5 mL). The mixture was heated at reflux for 1 h, cooled to room temperature, concentrated in vacuo. The resulting white solid was dissolved in EtOAc, washed with saturated aqueous NaHCO3, dried over Na2SO4 and concentrated to give compound 25 (660 mg, 99%) as a light yellow solid. 1H NMR (400 MHz, CDCl3) δ7.40 (d, 1H, J=7.2 Hz), 7.09 (d, 1H, J=10.0 Hz), 4.48 (br s, 2H).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 1 h
  3. concentrationconcentrated in vacuo
  4. dissolutionThe resulting white solid was dissolved in EtOAc
  5. washwashed with saturated aqueous NaHCO3
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0280bbb772fb42539330de233add3d48
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09216957B2

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