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Sulfuric Acid → HCID 14052571、化合物

HRID 330080
ノート
印刷プレビュー

反応式

HRID 330080 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]([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]
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 140525702,4,5-Trifluoro-3-methylbenzoyl chloride

生成物 1

HCID 14052571HCID 14052571、化合物収率 112.7%

試薬・触媒・溶媒 3

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0b1f87e24368493586440c74790c866e
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04894458

反応ノート

読み込み中…

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