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

HRID 1504945ノート

反応式

HRID 1504945 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0280bbb772fb42539330de233add3d48
出典データセット
uspto-grants-2015_12
特許番号
US09216957B2

反応ノート

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