Sodium Hydroxide → HCID 14257103、化合物

HRID 622110

反応式

HRID 622110 の反応式
[C:1]([C:6]1[N:10]([CH3:11])[C:9]([S:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[N:8][C:7]=1[CH3:22])(OCC)=[O:2].[H-].[Al+3].[H-].[H-].[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].[OH-].[Na+]>CCOCC.O>[CH3:11][N:10]1[C:6]([CH2:1][OH:2])=[C:7]([CH3:22])[N:8]=[C:9]1[S:12][CH2:13][C:14]1[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=1

参加物

8

反応物 5

HCID 14798Sodium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 14257102HCID 14257102、化合物HCID 21226445Aluminium lithium hydrideHCID 21584524Aluminiumhydride2 回

生成物 1

HCID 14257103HCID 14257103、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒4 回

反応条件

温度
0 °C

実験手順

5-Carbethoxy-1,4-dimethyl-2-(4-methoxybenzylthio)imidazole (31 g, 0.1 mole) dissolved in ether (250 ml) was added dropwise to a solution of aluminum hydride in ether stirred at 0° C. [the aluminum hydride in ether was prepared by adding lithium aluminum hydride (7.4 g, 0.19 mole) in portions to a solution of aluminum chloride (8.6 g, 0.065 mole) stirred in ether (200 ml) at 0° C⟧ The mixture was stirred at 0° C. for 1 hour, treated with water and 10% aqueous sodium hydroxide, filtered and concentrated in vacuo. The resulting oil was dissolved in methylene chloride, dried with magnesium sulfate, filtered and concentrated in vacuo to give 1,4-dimethyl-5-hydroxymethyl-2-(4-methoxybenzylthio)imidazole.

後処理

  1. customwas prepared
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. dissolutionThe resulting oil was dissolved in methylene chloride
  5. dry with materialdried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-6a7dc7cd8ded4a3c9867fe85a2edfb94
出典データセット
uspto-grants-1988_09
特許番号
US04769386

関連ノート

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