3-(2-Trifluoromethylphenyl)pentanedioic acid → 4-[2-(Trifluoromethyl)phenyl]oxane-2,6-dione

HRID 406376노트

반응식

HRID 406376 반응식
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]([CH2:14][C:15]([OH:17])=[O:16])[CH2:10][C:11](O)=[O:12]>C(OC(=O)C)(=O)C>[F:1][C:2]([F:19])([F:18])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH:9]1[CH2:14][C:15](=[O:17])[O:16][C:11](=[O:12])[CH2:10]1

참가 물질

3

반응물 1

HCID 666189203-(2-Trifluoromethylphenyl)pentanedioic acid

생성물 1

HCID 866626534-[2-(Trifluoromethyl)phenyl]oxane-2,6-dione수율 56.7%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

반응 조건

온도
110 °C

실험 절차

3-(2-Trifluoromethylphenyl)pentanedioic acid (1.2 g) was dissolved in acetic anhydride (12 mL), and the mixture was stirred at 110° C. for two hours. The oil after concentration under reduced pressure was dissolved in ethyl acetate and washed with a saturated sodium bicarbonate solution and brine. After drying over magnesium sulfate, concentration under reduced pressure gave an orange solid. The solid was recrystallized from ethyl acetate (10 mL) and heptane (70 mL) to obtain the title compound (636 mg) as a white powder.

후처리

  1. concentrationThe oil after concentration under reduced pressure
  2. dissolutionwas dissolved in ethyl acetate
  3. washwashed with a saturated sodium bicarbonate solution and brine
  4. dry with materialAfter drying over magnesium sulfate, concentration under reduced pressure
  5. customgave an orange solid
  6. customThe solid was recrystallized from ethyl acetate (10 mL) and heptane (70 mL)

출처 및 근거

ORD 기록
ord-8ee7f67ec2964ad59d06b3f81aeb9726
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754100B2

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