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

HRID 856762

반응식

HRID 856762 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae67017008b04a2f986cd7277017ef2c
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262185B2

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