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Sodium Dithionite → 3-Isobutyl-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]aniline

HRID 2388624
ノート
印刷プレビュー

反応式

HRID 2388624 の反応式
[CH2:1]([C:5]1[CH:6]=[C:7]([CH:9]=[CH:10][CH:11]=1)[NH2:8])[CH:2]([CH3:4])[CH3:3].[F:12][C:13]([F:22])([F:21])[C:14](I)([F:19])[C:15]([F:18])([F:17])[F:16].C(=O)([O-])O.[Na+].S(S([O-])=O)([O-])=O.[Na+].[Na+]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.CCCCCC.COC(C)(C)C.O>[CH2:1]([C:5]1[CH:6]=[C:7]([CH:9]=[CH:10][C:11]=1[C:14]([F:19])([C:15]([F:18])([F:17])[F:16])[C:13]([F:22])([F:21])[F:12])[NH2:8])[CH:2]([CH3:4])[CH3:3]
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 24489Sodium DithioniteHCID 33978Perfluoroisopropyl iodideHCID 516892Sodium BicarbonateHCID 190247993-Isobutylaniline

生成物 1

HCID 866190023-Isobutyl-4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]aniline収率 47%

試薬・触媒・溶媒 3

HCID 94433
Tetrabutylammonium hydrogen sulfate
触媒
HCID 8058Hexane溶媒
HCID 23212559water MeOtBu溶媒

実験手順

3-Isobutylaniline (14.9 g, 0.1 mol) was diluted in a 300 ml mixed solvent of tert-butyl methyl ether-water (1:1), followed by sequentially adding heptafluoroisopropyl iodide (29.6 g, 0.1 mol), tetrabutylammonium hydrogensulfate (3.4 g, 0.01 mol), sodium hydrogen carbonate (8.4 g, 0.1 mol) and sodium dithionite (17 g, 0.1 mol) and stirring overnight at room temperature. The reaction solution was diluted with hexane, followed by washing twice with a 3N HCl solution, and with aqueous sodium bicarbonate and a saturated brine. The solution was dried over magnesium sulfate and concentrated under reduced pressure, and then the residue was purified by using silica gel chromatography (hexane:ethyl acetate=6:1) to obtain 14.9 g of the desired compound.

後処理

  1. washby washing twice with a 3N HCl solution
  2. dry with materialThe solution was dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customthe residue was purified

出典と根拠

ORDレコード
ord-482b76009f7c40fcaf28a98a30b9208a
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08269045B2

反応ノート

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