Sulfuric Acid → 2-Iodo-4-(trifluoromethoxy)phenol

HRID 46306

반응식

HRID 46306 반응식
[I:1]N1C(=O)CCC1=O.[F:9][C:10]([F:20])([F:19])[O:11][C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1.S(=O)(=O)(O)O>C(O)(=O)C.O>[I:1][C:14]1[CH:13]=[C:12]([O:11][C:10]([F:19])([F:20])[F:9])[CH:17]=[CH:16][C:15]=1[OH:18]

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 70015p-(Trifluoromethoxy)phenolHCID 120273N-Iodosuccinimide

생성물 1

HCID 27694112-Iodo-4-(trifluoromethoxy)phenol수율 94%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

To a suspension of N-iodosuccinimide (6.95 g, 31 mmol) in glacial acetic acid (2 ml) was added 4-trifluoromethoxy phenol (4.0 ml, 31 mmol) and, after 5 minutes, concentrated sulphuric acid (0.5 ml, 9 mmol). The pale brown suspension was stirred at room temperature under nitrogen for 48 hours before diluting with water and extracting with dichloromethane. Organic extract was washed with water, saturated aqueous sodium thiosulphate solution, water, dried over magnesium sulfate and decolourising charcoal added. The resulting suspension was left to stand for 30 minutes before filtering through a short pad of silica gel eluting with dichloromethane. The solvent was evaporated in vacuo to give the title compound as an oil, 8.78 g, 94% yield.

후처리

  1. extractionextracting with dichloromethane
  2. extractionOrganic extract
  3. washwas washed with water, saturated aqueous sodium thiosulphate solution, water
  4. dry with materialdried over magnesium sulfate
  5. additionadded
  6. waitThe resulting suspension was left
  7. waitto stand for 30 minutes
  8. filtrationbefore filtering through a short pad of silica gel eluting with dichloromethane
  9. customThe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-ed5b836a8b304d37a4e16c36dca41b8e
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541588B2

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