Sulfuric Acid → HCID 23195887, 화합물

HRID 2209988노트

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HRID 2209988 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]([C:23]([F:26])([F:25])[F:24])=[C:21]([F:27])[CH:20]=[C:19]([F:28])[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>[F:13][C:14]1[C:22]([C:23]([F:24])([F:26])[F:25])=[C:21]([F:27])[CH:20]=[C:19]([F:28])[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

8

반응물 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 19035210HCID 19035210, 화합물

생성물 1

HCID 23195887HCID 23195887, 화합물

시약·촉매·용매 3

HCID 5943Carbon Tetrachloride촉매HCID 702Ethanol용매2회HCID 1140Toluene용매2회

실험 절차

0.58 g (0.024 mol) of magnesium filings are introduced into 1.3 ml of ethanol, the reaction is started up using a few drops of carbon tetrachloride, and a solution of 3.4 g (0,019 mol) of diethyl malonate in 2.4 ml of ethanol and 9 ml of toluene is subsequently added dropwise in such a manner that the internal temperature is between 50° and 60° C. Stirring is then continued for one hour at 60° C. A solution of 5.8 g (0,027 mol) of 2,4,6-trifluoro-3-trifluoromethylbenzoylchloride in 2.5 ml of toluene is added dropwise at -10 to -5° C., and stirring is continued for one hour at 0° C. and subsequently while the mixture comes to room temperature. The batch is poured into 10 ml of ice-water, treated with 1.5 ml of concentrated sulphuric acid, and the mixture is extracted using toluene. The toluene phase is washed using saturated sodium chloride solution, and the solvent is removed in vacuo.

후처리

  1. customis between 50° and 60° C
  2. stirringstirring
  3. waitis continued for one hour at 0° C. and subsequently while the mixture
  4. customcomes to room temperature
  5. extractionthe mixture is extracted
  6. washThe toluene phase is washed
  7. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-e2150a914032481fba6e48601b281a5a
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05457104

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