p-Toluenesulfonic acid → Ethyl (3,4,6-Trifluoro-2-methylbenzoyl)acetate

HRID 864331

反応式

HRID 864331 の反応式
[CH3:1][C:2]1[C:20]([F:21])=[C:19]([F:22])[CH:18]=[C:17]([F:23])[C:3]=1[C:4]([CH:6](C(OCC)=O)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].C1(C)C=CC(S(O)(=O)=O)=CC=1>O>[CH3:1][C:2]1[C:20]([F:21])=[C:19]([F:22])[CH:18]=[C:17]([F:23])[C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 17879412Diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate

生成物 1

HCID 14517129Ethyl (3,4,6-Trifluoro-2-methylbenzoyl)acetate収率 82.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate (5.1 g) are added water (20 ml) and p-toluenesulfonic acid (30 mg) and the mixture is refluxed for 2.5 hours. After cooling, the resultant is extracted with diethyl ether, and the extract is dried over magnesium sulfate and concentrated to give ethyl 2-methyl-3,4,6-trifluorobenzoylacetate (3.3 g).

後処理

  1. temperaturethe mixture is refluxed for 2.5 hours
  2. temperatureAfter cooling
  3. extractionthe resultant is extracted with diethyl ether
  4. dry with materialthe extract is dried over magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-a94c861ac06a4738b55bd7549e2d89d8
出典データセット
uspto-grants-1996_10
特許番号
US05563138

関連ノート

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