Water → 4-Ethylbenzo[d]oxazol-5-amine

HRID 1872785노트

반응식

HRID 1872785 반응식
[CH2:1]([C:3]1[C:8]2[N:9]=[CH:10][O:11][C:7]=2[CH:6]=[CH:5][C:4]=1[NH:12]C(=O)C(F)(F)F)[CH3:2].O.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CO>[NH2:12][C:4]1[CH:5]=[CH:6][C:7]2[O:11][CH:10]=[N:9][C:8]=2[C:3]=1[CH2:1][CH3:2]

참가 물질

6

반응물 4

HCID 962Water2회HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 154801414-Ethyl-5-trifluoroacetamidobenzoxazole

생성물 1

HCID 154801424-Ethylbenzo[d]oxazol-5-amine

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
90 °C

실험 절차

A solution of 4-ethyl-5-trifluoroacetamidobenzoxazole (14.13 mmol) in a 20% mixture of water in methanol (20 mL) is treated with anhydrous potassium carbonate (56.52 mmol). A reflux condenser is attached and the mixture is heated to 90° C. with an oil bath for five hours. The mixture is cooled to room temperature and distributed between ethyl acetate (100 mL) and water (100 mL). The ethyl acetate layer is dried over magnesium sulfate and concentrated under reduced pressure to yield a black residue. This material is purified by chromatography (silica gel, 50% ethyl acetate/hexanes) to afford 5-amino-4-ethylbenzoxazole.

후처리

  1. customA reflux condenser is attached
  2. temperatureThe mixture is cooled to room temperature
  3. dry with materialThe ethyl acetate layer is dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto yield a black residue
  6. customThis material is purified by chromatography (silica gel, 50% ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-dd41e73abcee457db3f9e19b0346cdc1
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06110952

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