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Sodium methanethiolate → 8-(2,6-Dimethylbenzylamino)-3-methyl-2-methylsulfanylmethyl-imidazo[1,2-a]pyridine

HRID 1006670
ノート
印刷プレビュー

反応式

HRID 1006670 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][S-:24].[Na+]>C(#N)C>[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][S: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

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 226726282-Chloromethyl-8-(2,6-dimethylbenzylamino)-3-methylimidazo[1,2-a]pyridine

生成物 1

HCID 226726258-(2,6-Dimethylbenzylamino)-3-methyl-2-methylsulfanylmethyl-imidazo[1,2-a]pyridine収率 24%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2-chloromethyl-8-(2,6-dimethylbenzylamino)-3-methylimidazo[1,2-a]pyridine (0.2 g, 0.64 mmol) and sodium methanethiolate (0.1 g, 1.3 mmol) were added to acetonitrile (10 ml) and stirred for 4 h. at room temperature. The solvent was evaporated under reduced pressure and to the residue were added methylene chloride and water. 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 (1:2) as eluent and crystallization from diethyl ether:petroleum ether (1:2) gave 0.05 g (24%) of the desired product.

後処理

  1. customThe solvent was evaporated under reduced pressure and to the residue
  2. additionwere added methylene chloride and water
  3. customThe organic layer was separated
  4. dry with materialdried (Na2SO4)
  5. customevaporated under reduced pressure
  6. customPurification of the residue by column chromatography on silica gel
  7. customcrystallization from diethyl ether:petroleum ether (1:2)

出典と根拠

ORDレコード
ord-dc8dd5d40e09446786402fc89e89795b
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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