Methylamine → 1-(6-Fluoropyridin-3-yl)-N-methylmethanamine

HRID 1585018ノート

反応式

HRID 1585018 の反応式
[CH3:1][NH2:2].[F:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10]Br)=[CH:6][CH:5]=1>CC#N>[F:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10][NH:2][CH3:1])=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 220506385-(Bromomethyl)-2-fluoropyridine

生成物 1

HCID 224503141-(6-Fluoropyridin-3-yl)-N-methylmethanamine収率 61%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a mixture of 2.5 g of 40% aqueous methylamine solution and 30 ml of CH3CN was added dropwise 3.0 g of crude (6-fluoro-3-pyridyl)methyl bromide with constant stirring. The mixture was allowed to stand at room temperature overnight and concentrated under reduced pressure. The residue was extracted with AcOEt and the extract was dried over MgSO4 and concentrated. The procedure gave 1.35 g of the title compound as a crude orange-colored oil.

後処理

  1. concentrationconcentrated under reduced pressure
  2. extractionThe residue was extracted with AcOEt
  3. dry with materialthe extract was dried over MgSO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-058e785b2242402ca630f02db8227006
出典データセット
uspto-grants-1999_08
特許番号
US05935981

反応ノート

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