Sulfuric Acid → Diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate

HRID 864330

반응식

HRID 864330 반응식
[Mg].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH3:13][C:14]1[C:22]([F:23])=[C:21]([F:24])[CH:20]=[C:19]([F:25])[C:15]=1[C:16](Cl)=[O:17].S(=O)(=O)(O)O>C(Cl)(Cl)(Cl)Cl.C(O)C.C1(C)C=CC=CC=1.O>[CH3:13][C:14]1[C:22]([F:23])=[C:21]([F:24])[CH:20]=[C:19]([F:25])[C:15]=1[C:16]([CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:2]([O:10][CH2:11][CH3:12])=[O:9])=[O:17]

참가 물질

9

반응물 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 150076072-Methyl-3,4,6-trifluorobenzoyl chloride

생성물 1

HCID 17879412Diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate

시약·촉매·용매 4

HCID 5943Carbon Tetrachloride촉매HCID 702Ethanol용매2회HCID 962Water용매HCID 1140Toluene용매2회

반응 조건

온도
60 °C

실험 절차

Separately, two drops of carbon tetrachloride are added to a solution of metallic magnesium (0.4 g) in absolute ethanol (0.9 ml). When the reaction starts, a mixture of diethyl malonate (2.6 ml), absolute ethanol (1.6 ml) and anhydrous toluene (6 ml) is added dropwise below 60° C. After stirring at 60° C. for 1 hour, the reaction mixture is cooled to 0° C. and thereto a solution of 2-methyl-3,4,6-trifluorobenzoyl chloride prepared above in toluene (5 ml) is added dropwise. After stirring for 30 minutes, a mixture of conc. sulfuric acid (0.4 ml) and water (6 ml) is added and the mixture is extracted with diethyl ether, and the extract is dried over magnesium sulfate and concentrated to give diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate (5.2 g).

후처리

  1. additionis added dropwise below 60° C
  2. temperaturethe reaction mixture is cooled to 0° C.
  3. additionis added dropwise
  4. stirringAfter stirring for 30 minutes
  5. additionis added
  6. extractionthe mixture is extracted with diethyl ether
  7. dry with materialthe extract is dried over magnesium sulfate
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9caa029acfe1496d9f01e34ec6b97123
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05563138

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