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Sulfuric Acid → HCID 14052571, 화합물

HRID 330080
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HRID 330080 반응식
[Mg].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[F:13][C:14]1[C:22]([CH3:23])=[C:21]([F:24])[C:20]([F:25])=[CH:19][C:15]=1[C:16](Cl)=[O:17].S(=O)(=O)(O)O>C1(C)C=CC=CC=1.C(O)C.C(Cl)(Cl)(Cl)Cl>[F:13][C:14]1[C:22]([CH3:23])=[C:21]([F:24])[C:20]([F:25])=[CH:19][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 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 140525702,4,5-Trifluoro-3-methylbenzoyl chloride

생성물 1

HCID 14052571HCID 14052571, 화합물수율 112.7%

시약·촉매·용매 3

HCID 702Ethanol용매2회
HCID 1140
Toluene
용매
2회
HCID 5943Carbon Tetrachloride용매

실험 절차

To a mixture of magnesium turnings (0.69 g) and absolute ethanol (4.7 ml) was added carbon tetrachloride (0.4 ml). To the stirring suspension was added a solution of diethyl malonate (4.41 g) and absolute ethanol (4.7 ml) in anhydrous toluene (19.2 ml) dropwise during 10 minutes at 15° to 50° C. After the mixture was stirred at 50° to 60° C. for 2 hours, to the mixture was added a solution of 2,4,5-trifluoro-3-methylbenzoyl chloride (4.51 g) in anhydrous toluene (6.4 ml) dropwise at -16° to -13° C. during 10 minutes. The reacting mixture was stirred at -20° C. for 1 hour, and then warmed gradually to room temperature during 1.5 hours with stirring. To this solution was added ice water (25 ml) containing concentrated sulfuric acid (0.8 ml), extracted with toluene. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium chloride and concentrated under reduced pressure to give the title compound (8.10 g).

후처리

  1. stirringThe reacting mixture was stirred at -20° C. for 1 hour
  2. stirringwith stirring
  3. extractionextracted with toluene
  4. washThe organic layer was washed with saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous sodium chloride
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0b1f87e24368493586440c74790c866e
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04894458

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