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Bromine → 2-Bromo-6-methoxypyridin-3-amine

HRID 12307
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HRID 12307 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1.C([O-])(=O)C.[Na+].[Br:15]Br.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(O)(=O)C>[NH2:1][C:2]1[C:7]([Br:15])=[N:6][C:5]([O:8][CH3:9])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 24408BromineHCID 24477Sodium ThiosulfateHCID 811216-Methoxy-3-pyridinylamineHCID 517045Sodium Acetate

생성물 1

HCID 152093242-Bromo-6-methoxypyridin-3-amine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 1.83 g (14.7 mM) of 5-amino-2-methoxypyridine and 1.21 g (14.7 mM) of sodium acetate in 12 ml of acetic acid is prepared and 0.75 ml (14.7 mM) of bromine is added gently, with stirring and while maintaining at room temperature. The reaction mixture is kept stirring for 30 minutes, at room temperature, and 200 ml of saturated sodium thiosulfate solution are then added. The aqueous phase obtained is extracted twice with ethyl acetate. The combined organic phases are dried over magnesium sulfate and concentrated under reduced pressure. 3 g of the expected compound are obtained in the form of a violet-colored solid (quantitative yield).

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후처리

  1. customis prepared
  2. stirringThe reaction mixture is kept stirring for 30 minutes, at room temperature
  3. customThe aqueous phase obtained
  4. extractionis extracted twice with ethyl acetate
  5. dry with materialThe combined organic phases are dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-27352282c0af4dfbb16addeee00b36b0
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07728002B2

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