Potassium Hydroxide → 2,4-Dichloro-5-methoxy-3-trifluoromethylaniline

HRID 409685ノート

反応式

HRID 409685 の反応式
[OH-].[K+].[Cl:3][C:4]1[C:9]([C:10]([F:13])([F:12])[F:11])=[C:8]([Cl:14])[C:7]([O:15][CH3:16])=[CH:6][C:5]=1[NH:17]C(=O)C>O.CCO>[Cl:3][C:4]1[C:9]([C:10]([F:13])([F:12])[F:11])=[C:8]([Cl:14])[C:7]([O:15][CH3:16])=[CH:6][C:5]=1[NH2:17]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 86625462N-(2,4-dichloro-5-methoxy-3-trifluoromethyl-phenyl)-acetamide

生成物 1

HCID 866254602,4-Dichloro-5-methoxy-3-trifluoromethylaniline

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A 2 M solution of KOH in water (1.87 mL) is added to a solution of N-(2,4-dichloro-5-methoxy-3-trifluoromethyl-phenyl)-acetamide (104 mg, 0.344 mmol) in EtOH (3 mL). After stirring for 3.5 h at 80° C. followed by cooling to RT, the solvent is evaporated and the residue is taken up in EtOAc and a saturated aqueous solution of NaHCO3. The separated aqueous layer is extracted twice with EtOAc. The organic phases are washed with brine, dried (Na2SO4), filtered and concentrated, providing the title compound: ESI-MS: 258/260 [M-H]−1; tR=4.8 min (system 1); TLC: Rf=0.54 (EtOAc).

後処理

  1. temperatureby cooling to RT
  2. customthe solvent is evaporated
  3. extractionThe separated aqueous layer is extracted twice with EtOAc
  4. washThe organic phases are washed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-9835d3d4c3ae44199156f49ba2c6c50b
出典データセット
uspto-grants-2014_06
特許番号
US08759517B2

反応ノート

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