Hydrochloric Acid → 4-Carboxy-5-hexyl-3-(2,6-difluorophenyl)isoxazole

HRID 434041노트

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HRID 434041 반응식
C[O:2][C:3]([C:5]1[C:6]([C:16]2[C:21]([F:22])=[CH:20][CH:19]=[CH:18][C:17]=2[F:23])=[N:7][O:8][C:9]=1[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])=[O:4].Cl>CO>[C:3]([C:5]1[C:6]([C:16]2[C:21]([F:22])=[CH:20][CH:19]=[CH:18][C:17]=2[F:23])=[N:7][O:8][C:9]=1[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])([OH:4])=[O:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 187562734-Methoxycarbonyl-5-hexyl-3-(2,6-difluorophenyl)isoxazole

생성물 1

HCID 187562704-Carboxy-5-hexyl-3-(2,6-difluorophenyl)isoxazole수율 77.2%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

4-Methoxycarbonyl-5-hexyl-3-(2,6-difluorophenyl)isoxazole (0.30 g, 0.88 mmol) was dissolved in methanol (10 ml), 5N NAOH (1 ml) was added, and the mixture was heated at 50° C. for 2 h. Upon cooling to room temperature, HCl was added until pH 1. Extraction with ethyl acetate and subsequent washing of the organic fraction (brine), drying (MgSO4), filtering, and concentrating afforded the desired 4-carboxy-5-hexyl-3-(2,6-difluorophenyl)isoxazole (0.21 g, 72%) that was used without further purification.

후처리

  1. addition5N NAOH (1 ml) was added
  2. temperatureUpon cooling to room temperature
  3. extractionExtraction with ethyl acetate
  4. washsubsequent washing of the organic fraction (brine)
  5. dry with materialdrying (MgSO4)
  6. filtrationfiltering
  7. concentrationconcentrating

출처 및 근거

ORD 기록
ord-b7efad12ae4b4bb780affa7107ff99ab
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06670373B1

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