Morpholine → (3-Chloro-4-morpholinopyridin-2-yl)methanol

HRID 1655208노트

반응식

HRID 1655208 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[Cl:7][C:8]1[C:9]([CH2:15][OH:16])=[N:10][CH:11]=[CH:12][C:13]=1Cl>C(O)C>[O:4]1[CH2:5][CH2:6][N:1]([C:13]2[CH:12]=[CH:11][N:10]=[C:9]([CH2:15][OH:16])[C:8]=2[Cl:7])[CH2:2][CH2:3]1

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 22117301(3,4-Dichloropyridin-2-yl)methanol

생성물 1

HCID 19791250(3-Chloro-4-morpholinopyridin-2-yl)methanol

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Morpholine (7.34 ml) and 3.4 -dichloro-2 -hydroxymethylpyridine (3.0 g) were heated together in a bomb at 180 ° for 4 hours. After cooling, the mixture was taken up in ethanol and evaporated under reduced pressure to remove excess amine. The residue was taken up in water and extracted with chloroform. After drying (K2CO3 ) and removal of solvent, the residue was chromatographed (silica gel, CHCl3) to give an oil which was crystallised from petroleum ether (60/80 ) to give 4 -morpholino-3 -chloro-2 -hydroxymethylpyridine, 3.24 g, m.p. 80°-2°.

후처리

  1. temperatureAfter cooling
  2. customevaporated under reduced pressure
  3. customto remove excess amine
  4. extractionextracted with chloroform
  5. customAfter drying
  6. custom(K2CO3 ) and removal of solvent
  7. customthe residue was chromatographed (silica gel, CHCl3)
  8. customto give an oil which
  9. customwas crystallised from petroleum ether (60/80 )

출처 및 근거

ORD 기록
ord-731ba16b5b2e4e72a148519e2fcef5de
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250527

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