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

HRID 2066715ノート

反応式

HRID 2066715 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]−; 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-ab4d52bfa130487eb70315afcfea4f21
出典データセット
uspto-grants-2012_10
特許番号
US08293746B2

反応ノート

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