Phosphorus oxychloride → 5-Methyl-2-pentyl-4-phenyl-1,3-oxazole

HRID 1982437ノート

反応式

HRID 1982437 の反応式
P(Cl)(Cl)(Cl)=O.[C:6]([NH:13][CH:14]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:15](=[O:17])[CH3:16])(=O)[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]>C1(C)C=CC=CC=1>[CH3:16][C:15]1[O:17][C:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])=[N:13][C:14]=1[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

4

反応物 2

HCID 24813Phosphorus oxychlorideHCID 13293301N-(2-Oxo-1-phenylpropyl)hexanamide

生成物 1

HCID 233165955-Methyl-2-pentyl-4-phenyl-1,3-oxazole

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Phosphorous oxychloride (5.58 ml) was added to a solution of 1-hexanoylamino-1-phenyl-2-propanone (4.94 g) in toluene (50 ml) and the solution was refluxed with stirring for 40 minutes. The solvent was distilled off and water was added to the residue. The mixture was neutralized with potassium carbonate and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was then distilled off and the residue was purified by silica gel chromatography [silice gel: 80 g; eluent: hexane-ethyl ether (4:1)] to give an oil of 5-methyl-2-pentyl-4-phenyloxazole, yield 4.25 g (92.8%).

後処理

  1. temperaturethe solution was refluxed
  2. distillationThe solvent was distilled off
  3. additionwater was added to the residue
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was then distilled off
  8. customthe residue was purified by silica gel chromatography [silice gel: 80 g; eluent: hexane-ethyl ether (4:1)]

出典と根拠

ORDレコード
ord-3af3bec9a2084cfabd07eed7aea8bb44
出典データセット
uspto-grants-1986_06
特許番号
US04596816

反応ノート

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