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Sulfuric Acid → HCID 22077298、化合物

HRID 2209986
ノート
印刷プレビュー

反応式

HRID 2209986 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]=[CH:19][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:25])[F:26])=[C:21]([F:27])[CH:20]=[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 19035209HCID 19035209、化合物

生成物 1

HCID 22077298HCID 22077298、化合物

試薬・触媒・溶媒 3

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

実験手順

2.15 g (0.09 mol) of magnesium filings are introduced into 4.8 ml of ethanol, the reaction is started up using a few drops of carbon tetrachloride, and a solution of 12.8 g (0.075 mol) of diethyl malonate in 9 ml of ethanol and 35 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 20.0 g (0.082 mol) of 2,4-difluoro-3-trifluoromethylbenzoyl chloride in 9 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 35 ml of ice-water, treated with 5.7 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-304a94b2b923489a98983ad1745a7540
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05457104

反応ノート

読み込み中…

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