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

HRID 1655208ノート

反応式

HRID 1655208 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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°.

後処理

  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 )

出典と根拠

ORDレコード
ord-731ba16b5b2e4e72a148519e2fcef5de
出典データセット
uspto-grants-1993_10
特許番号
US05250527

反応ノート

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