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

HRID 409685노트

반응식

HRID 409685 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9835d3d4c3ae44199156f49ba2c6c50b
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759517B2

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