Potassium Hydroxide → 3-(4-Ethyl-2-methoxyphenoxy)-2-nitropyridine

HRID 626005

반응식

HRID 626005 반응식
F[C:2]1[C:3]([N+:8]([O-:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.[CH2:11]([C:13]1[CH:18]=[CH:17][C:16]([OH:19])=[C:15]([O:20][CH3:21])[CH:14]=1)[CH3:12].[OH-].[K+]>C(#N)C>[CH2:11]([C:13]1[CH:18]=[CH:17][C:16]([O:19][C:2]2[C:3]([N+:8]([O-:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=2)=[C:15]([O:20][CH3:21])[CH:14]=1)[CH3:12]

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 624654-EthylguaiacolHCID 27628023-Fluoro-2-nitropyridine

생성물 1

HCID 591912683-(4-Ethyl-2-methoxyphenoxy)-2-nitropyridine수율 84.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

반응 조건

온도
80 °C

실험 절차

To a stirred solution of 3-Fluoro 2-nitro pyridine (1.6 g, 0.01126 mol) in dry Acetonitrile (20 ml) was added 4-Ethyl-2-methoxy phenol (1.71 g, 11.3 mmol) in dry acetonitrile (10 ml) followed by potassium hydroxide (0.696 g, 12.4 mmol). The reaction mixture was heated to 80° C. and maintained for 2 hours. The solvent was evaporated and taken in ethyl acetate (200 ml). The organic layer was washed with water followed by brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 2.6 g of crude product purified by column chromatography (5% Ethyl acetate in Petroleum ether) to yield: 1.75 g (56%) of title compound.

후처리

  1. temperaturemaintained for 2 hours
  2. customThe solvent was evaporated
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0134fb5f56ae4a8e9368241693265e86
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309179B2

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