Water → 5-Bromo-N-methylpyridin-2-amine

HRID 268963ノート

反応式

HRID 268963 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5](F)=[N:6][CH:7]=1.[CH3:9][NH2:10].O>C1COCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:10][CH3:9])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 6329MethylamineHCID 27831685-Bromo-2-fluoropyridine

生成物 1

HCID 156456635-Bromo-N-methylpyridin-2-amine収率 24%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 5-bromo-2-fluoropyridine (2.5 g, 14 mmol) in THF (50 mL) was stirred with a solution of methylamine in THF (c=2 mol/L) (35 mL, 70 mmol) at 23° C. for 16 h. Water was added and the mixture was extracted with ether, the organic layer was dried over Na2SO4. Removal of the solvent in vacuum left a residue which was purified by silica gel column chromatography with heptane/ether, followed by trituration with heptane to give the title compound as a white solid (630 mg, 24%). MS (ISP) 187.1 [(M+H)+], 189.2 [(M+2+H)+].

後処理

  1. extractionthe mixture was extracted with ether
  2. dry with materialthe organic layer was dried over Na2SO4
  3. customRemoval of the solvent in vacuum
  4. waitleft a residue which
  5. customwas purified by silica gel column chromatography with heptane/ether

出典と根拠

ORDレコード
ord-e6696ee166944486ba6ca70669f0c348
出典データセット
uspto-grants-2008_11
特許番号
US07446113B2

反応ノート

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