Calcium hypochlorite → 5-Propionyl-3-phenylisoxazole

HRID 345178

반응식

HRID 345178 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 151807665-Propionyl-3-phenylisoxazole

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eb37384716134ff39c15317a1454392c
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05055585

연결된 노트

불러오는 중…