Toluene → 2-Bromo-1-[3-(trifluoromethyl)phenyl]ethan-1-one

HRID 229730

反応式

HRID 229730 の反応式
C1(C)C=CC=CC=1.[F:8][C:9]([F:20])([F:19])[C:10]1[CH:11]=[C:12]([C:16](=[O:18])[CH3:17])[CH:13]=[CH:14][CH:15]=1.C1C=C[NH+]=CC=1.[Br:27][Br-]Br>O>[Br:27][CH2:17][C:16]([C:12]1[CH:13]=[CH:14][CH:15]=[C:10]([C:9]([F:19])([F:20])[F:8])[CH:11]=1)=[O:18]

参加物

4

反応物 2

HCID 1140TolueneHCID 676823'-(Trifluoromethyl)acetophenone

生成物 1

HCID 27783862-Bromo-1-[3-(trifluoromethyl)phenyl]ethan-1-one収率 81.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a toluene solution (423 mL) of commercially available 3′-trifluoromethylacetophenone (79.6 g, 0.423 mol) was added pyridinium bromide perbromide (135.4 g, 0.423 mol) under ice cooling and stirred for 5 hours while heating up to room temperature. The reaction liquid was ice cooled again, followed by dropwise adding 400 mL of distilled water to stop reaction and fractionation. A toluene layer was washed with 400 mL of a saturated aqueous solution of sodium bicarbonate, followed by drying with magnesium sulfate anhydride and concentration under reduced pressure and distillation under reduced pressure to obtain an objective compound (92.35 g, 81.7%).

後処理

  1. customThe reaction liquid
  2. temperaturecooled again
  3. customreaction and fractionation
  4. washA toluene layer was washed with 400 mL of a saturated aqueous solution of sodium bicarbonate
  5. dry with materialby drying with magnesium sulfate anhydride and concentration under reduced pressure and distillation under reduced pressure

出典と根拠

ORDレコード
ord-1563afc41a58401c95a39af9048a3f05
出典データセット
uspto-grants-2009_07
特許番号
US07563893B2

関連ノート

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