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Morpholine → 4-(5-bromopyridin-2-yl)morpholine

HRID 1021267
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HRID 1021267 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5](Cl)=[N:6][CH:7]=1.[NH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1>CN(C)C(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[N:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 8083MorpholineHCID 27344145-Bromo-2-chloropyridine

생성물 1

HCID 109667244-(5-bromopyridin-2-yl)morpholine

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
130 °C

실험 절차

5-Bromo-2-chloropyridine (5.0 g) was mixed with N,N-dimethylacetamide (25 ml), and morpholine (23 ml) was added thereto, followed by stirring at 130° C. for 2 days. The reaction mixture was concentrated under reduced pressure, and water was added to the residue, followed by extraction with EtOAc, and the organic layer was washed with saturated brine and dried over Na2SO4. The organic layer was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/EtOAc) to obtain 4-(5-bromopyridin-2-yl)morpholine (6.07 g).

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후처리

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and water
  3. additionwas added to the residue
  4. extractionfollowed by extraction with EtOAc
  5. washthe organic layer was washed with saturated brine
  6. dry with materialdried over Na2SO4
  7. concentrationThe organic layer was concentrated under reduced pressure
  8. customThe obtained residue was purified by silica gel column chromatography (hexane/EtOAc)

출처 및 근거

ORD 기록
ord-bafc666d8c6c4fd09f3405f2b9654f78
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716470B2

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