Iodine → 2-Iodo-6-(trifluoromethyl)pyridin-3-amine

HRID 12306노트

반응식

HRID 12306 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([F:11])([F:10])[F:9])=[N:6][CH:7]=1.[I:12]I>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[NH2:1][C:2]1[C:7]([I:12])=[N:6][C:5]([C:8]([F:11])([F:9])[F:10])=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 807IodineHCID 27377445-Amino-2-(trifluoromethyl)pyridine

생성물 1

HCID 534254792-Iodo-6-(trifluoromethyl)pyridin-3-amine수율 96%

시약·촉매·용매 2

HCID 178418844HCID 178418844, 화합물촉매HCID 702Ethanol용매

실험 절차

3.85 g (12.3 mM) of silver sulfate are added, with stirring and at room temperature, to a solution of 2 g (12.3 mM) of 5-amino-2-(trifluoromethyl)pyridine in 100 ml of ethanol. 3.13 g of iodine are then added and the reaction mixture is stirred at room temperature for 24 hours. The solid in suspension in the medium is removed by filtration and the filtrate is concentrated under reduced pressure. The evaporation residue is taken up in 200 ml of dichloromethane and washed with 5% sodium hydroxide solution, and then with water and dried over magnesium sulfate. The solution obtained is concentrated under reduced pressure and 3.42 g of the expected compound are thus obtained in the form of a pink solid (yield=96%).

후처리

  1. customThe solid in suspension in the medium is removed by filtration
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. washwashed with 5% sodium hydroxide solution
  4. dry with materialwith water and dried over magnesium sulfate
  5. customThe solution obtained
  6. concentrationis concentrated under reduced pressure and 3.42 g of the expected compound

출처 및 근거

ORD 기록
ord-d8ab2f2da6704ce983b0aa772fa77a07
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728002B2

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