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Methanol → 8-(2,6-Dimethylbenzylamino)-2-methoxymethyl-3-methyl-imidazo[1,2-a]pyridine

HRID 1006671
ノート
印刷プレビュー

反応式

HRID 1006671 の反応式
Cl[CH2:2][C:3]1[N:4]=[C:5]2[C:10]([NH:11][CH2:12][C:13]3[C:18]([CH3:19])=[CH:17][CH:16]=[CH:15][C:14]=3[CH3:20])=[CH:9][CH:8]=[CH:7][N:6]2[C:21]=1[CH3:22].[CH3:23][OH:24]>>[CH3:20][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]([CH3:19])[C:13]=1[CH2:12][NH:11][C:10]1[C:5]2[N:6]([C:21]([CH3:22])=[C:3]([CH2:2][O:24][CH3:23])[N:4]=2)[CH:7]=[CH:8][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 887MethanolHCID 226726282-Chloromethyl-8-(2,6-dimethylbenzylamino)-3-methylimidazo[1,2-a]pyridine

生成物 1

HCID 185164128-(2,6-Dimethylbenzylamino)-2-methoxymethyl-3-methyl-imidazo[1,2-a]pyridine収率 44%

実験手順

2-chloromethyl-8-(2,6-dimethylbenzylamino)-3-methylimidazo[1,2-a]pyridine (0.3 g, 0.96 mmol) was solved in methanol (20 ml) and stirred for 20 h. at room temperature and refluxed for 20 min. The solvent was evaporated under reduced pressure and the residue was dissolved in methylene chloride and washed with a bicarbonate solution. The organic layer was separated, dried (Na2SO4) and evaporated under reduced pressure. Purification of the residue by column chromatography on silica gel using diethyl ether:petroleum ether (2:1) as eluent and crystallization from diethyl ether:petroleum ether (2:1) gave 0.13 g (44%) of the desired product.

後処理

  1. temperaturerefluxed for 20 min
  2. customThe solvent was evaporated under reduced pressure
  3. dissolutionthe residue was dissolved in methylene chloride
  4. washwashed with a bicarbonate solution
  5. customThe organic layer was separated
  6. dry with materialdried (Na2SO4)
  7. customevaporated under reduced pressure
  8. customPurification of the residue by column chromatography on silica gel
  9. customcrystallization from diethyl ether:petroleum ether (2:1)

出典と根拠

ORDレコード
ord-5c917d510df340b39d88ede126819282
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06790960B2

反応ノート

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