Hydrochloric Acid → 5-Ethyl-1,3-benzoxazol-2(3H)-one

HRID 2253569노트

반응식

HRID 2253569 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([CH2:8][CH3:9])[CH:5]=[CH:4][C:3]=1[OH:10].N[C:12](N)=[O:13].Cl>>[CH2:8]([C:6]1[CH:5]=[CH:4][C:3]2[O:10][C:12](=[O:13])[NH:1][C:2]=2[CH:7]=1)[CH3:9]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 1176UreaHCID 7218852-Amino-4-ethylphenol

생성물 1

HCID 197458335-Ethyl-1,3-benzoxazol-2(3H)-one수율 60.5%

반응 조건

온도
180 °C

실험 절차

8.2 g (0.06 M) 2-amino-4-ethylphenol and 5.4 g (0.09 M) urea were thoroughly mixed and heated in an oil bath to 180° C. for 2.0 hours. Thereafter the mixture was allowed to cool to 100° C. HCl solution (1.0 normal) was added to the mixture while stirring and the mixture was cooled to room temperature. The cooled mixture was extracted three times with methylene chloride. The combined organic phases were dried and stripped in vacuum. The sample yielded 5.9 g dark solid with a melting point of 75°-77° C. Spectroscopic data: nuclear magnetic resonance (NMR), C-13 NMR, infrared, and mass spectroscopy are consistent with the proposed structure.

후처리

  1. temperatureto cool to 100° C
  2. temperaturethe mixture was cooled to room temperature
  3. extractionThe cooled mixture was extracted three times with methylene chloride
  4. customThe combined organic phases were dried

출처 및 근거

ORD 기록
ord-67e13d2a0c1e4ccaae63f5a85b478ea4
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05232899

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