Calcium hypochlorite → 5-Propionyl-3-phenylisoxazole

HRID 345178

反応式

HRID 345178 の反応式
[OH:1][CH:2]([C:5]1[O:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=1)[CH2:3][CH3:4].Cl.N1C=CC=CC=1.Cl[O-].[Ca+2].Cl[O-]>ClCCl>[C:2]([C:5]1[O:9][N:8]=[C:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:6]=1)(=[O:1])[CH2:3][CH3:4]

参加物

5

反応物 3

HCID 24504Calcium hypochloriteHCID 10176127Pyridinium chlorideHCID 151807655-(1-Hydroxypropyl)-3-phenylisoxazole

生成物 1

HCID 151807665-Propionyl-3-phenylisoxazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 10 ml of dichloromethane, 1.0 g (5.0 mmol) of 5-(1-hydroxypropyl)-3-phenylisoxazole was dissolved. To the solution were added 100 mg (0.9 mmol) of pyridine hydrochloride, followed by the further addition of 1.4 g (9.9 mmol) of calcium hypochlorite. They were reacted at room temperature for 5 hours. After completion of the reaction, insoluble matter was filtered off and the organic layer was washed with water. The organic layer was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was then recrystallized from ethanol, whereby the target compound, namely, 5-propionyl-3-phenylisoxazole was obtained as crystals.

後処理

  1. customThey were reacted at room temperature for 5 hours
  2. customAfter completion of the reaction, insoluble matter
  3. filtrationwas filtered off
  4. washthe organic layer was washed with water
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was then recrystallized from ethanol, whereby the target compound

出典と根拠

ORDレコード
ord-eb37384716134ff39c15317a1454392c
出典データセット
uspto-grants-1991_10
特許番号
US05055585

関連ノート

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