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Tin tetrachloride dihydrate → HCID 178507836, 화합물

HRID 1943758
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HRID 1943758 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([OH:8])[C:3]=1[N+:9]([O-])=O.O.O.[Sn](Cl)(Cl)(Cl)Cl>C(O)C>[NH2:9][C:3]1[C:4]([OH:8])=[N:5][CH:6]=[CH:7][C:2]=1[Cl:1]
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참가 물질

4

반응물 2

HCID 85782573Tin tetrachloride dihydrateHCID 178526742HCID 178526742, 화합물

생성물 1

HCID 178507836HCID 178507836, 화합물수율 46.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-chloro-3-nitro-pyridin-2-ol (1.69 g, 9.72 mmol) and tin tetrachloride dihydrate (SnCl2.2H2O) (10.97 g, 48.62 mmol) was dissolved in ethanol (32 ml), heated to 70□ and stirred for 2 hours. The reaction mixture was cooled to room temperature and the ethanol was evaporated under reduced pressure. The residue was neutralized with saturated aqueous solution of sodium hydrogen carbonate, and extracted with ethyl acetate. The combined organic layer was washed with water and saturated saline solution, dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain pale-yellow solid (650 mg, 46%).

후처리

  1. temperatureheated to 70□
  2. customthe ethanol was evaporated under reduced pressure
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layer was washed with water and saturated saline solution
  5. dry with materialdried over anhydrous sodium sulfate (Na2SO4)
  6. filtrationfiltered
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-25890cb29281430dab1148d418f157c6
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08394792B2

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