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

HRID 406376ノート

反応式

HRID 406376 の反応式
[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

参加物

3

反応物 1

HCID 666189203-(2-Trifluoromethylphenyl)pentanedioic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8ee7f67ec2964ad59d06b3f81aeb9726
出典データセット
uspto-grants-2014_06
特許番号
US08754100B2

反応ノート

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