Water → 3-Methyl-4-[[(1-methylimidazol-2-yl)methyl]sulfanyl]aniline

HRID 856762

反応式

HRID 856762 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[C:4]([CH3:9])[CH:3]=1.[OH-].[Na+].Cl.Cl[CH2:14][C:15]1[N:16]([CH3:20])[CH:17]=[CH:18][N:19]=1.O>CO>[CH3:9][C:4]1[CH:3]=[C:2]([CH:7]=[CH:6][C:5]=1[S:8][CH2:14][C:15]1[N:16]([CH3:20])[CH:17]=[CH:18][N:19]=1)[NH2:1]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 27954062-(chloromethyl)-1-methyl-1H-imidazole hydrochlorideHCID 198673854-Amino-2-methylbenzene-1-thiol

生成物 1

HCID 433031753-Methyl-4-[[(1-methylimidazol-2-yl)methyl]sulfanyl]aniline収率 90.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 4-amino-2-methylthiophenol (500 mg) in methanol (10 ml) was added 1N aqueous solution of sodium hydroxide (12 ml), and a solution of 2-chloromethyl-1-methylimidazole hydrochloride (660 mg) in methanol (10 ml) was added at 0° C. Water was added to the mixture, and the mixture was extracted with ethyl acetate and the organic layer was dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was recrystallized from hexane-ethyl acetate, to give 3-methyl-4-[[(1-methylimidazol-2-yl)methyl]sulfanyl]aniline (757 mg) as crystals.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe obtained residue was recrystallized from hexane-ethyl acetate

出典と根拠

ORDレコード
ord-ae67017008b04a2f986cd7277017ef2c
出典データセット
uspto-grants-2007_08
特許番号
US07262185B2

関連ノート

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