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Methyl iodide → 3-Bromo-5-ethyl-6-methoxy-2-methylpyridine

HRID 1921307
ノート
印刷プレビュー

反応式

HRID 1921307 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][CH3:11])[C:5](=[O:9])[NH:6][C:7]=1[CH3:8].IC.Cl[CH2:15]Cl>[Al].C(=O)([O-])[O-].[Ag+2]>[Br:1][C:2]1[C:7]([CH3:8])=[N:6][C:5]([O:9][CH3:15])=[C:4]([CH2:10][CH3:11])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodide2 回HCID 6344DichloromethaneHCID 207792745-bromo-3-ethyl-6-methyl-1H-pyridin-2-one

生成物 1

HCID 116586693-Bromo-5-ethyl-6-methoxy-2-methylpyridine収率 99.9%

試薬・触媒・溶媒 2

HCID 178418647HCID 178418647、化合物触媒HCID 5359268
Aluminum
溶媒

実験手順

A mixture of 5-bromo-3-ethyl-6-methyl-1H-pyridin-2-one (41.8 g, 0.193 mol) obtained from Step 2 as described above, iodomethane (70 mL, 1.12 mol), silver carbonate (72 g, 0.261 mol) and dichloromethane is mechanically stirred at ambient temperature for 17 hr (The reaction vessel is wrapped in aluminum foil). An additional portion of iodomethane (70 mL, 1.12 mol) is added and stirring continued for an additional 20 hr. The reaction mixture is filtered through a pad of Celite and the filter cake is washed with dichloromethane. The combined filtrate and wash is concentrated to afford the title compound (44.35 g, 99.9% yield) as a yellow oil.

後処理

  1. stirringstirring
  2. waitcontinued for an additional 20 hr
  3. filtrationThe reaction mixture is filtered through a pad of Celite
  4. washthe filter cake is washed with dichloromethane
  5. washThe combined filtrate and wash
  6. concentrationis concentrated

出典と根拠

ORDレコード
ord-79397737d65c4134aa19e45d8cb77e6c
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08173682B2

反応ノート

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