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

HRID 2253569ノート

反応式

HRID 2253569 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
180 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-67e13d2a0c1e4ccaae63f5a85b478ea4
出典データセット
uspto-grants-1993_08
特許番号
US05232899

反応ノート

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