Sulfuric Acid → HCID 23195887、化合物

HRID 2209988ノート

反応式

HRID 2209988 の反応式
[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]

参加物

8

反応物 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 19035210HCID 19035210、化合物

生成物 1

HCID 23195887HCID 23195887、化合物

試薬・触媒・溶媒 3

HCID 5943Carbon Tetrachloride触媒HCID 702Ethanol溶媒2 回HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e2150a914032481fba6e48601b281a5a
出典データセット
uspto-grants-1995_10
特許番号
US05457104

反応ノート

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