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

HRID 229730

반응식

HRID 229730 반응식
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]

참가 물질

4

반응물 2

HCID 1140TolueneHCID 676823'-(Trifluoromethyl)acetophenone

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-1563afc41a58401c95a39af9048a3f05
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563893B2

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