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Acetonitrile → 2-Chloro-1-[2-hydroxy-2-methyl-3-(4-methylbenzenesulfonyloxy)propyl]-4-nitroimidazole

HRID 856148
ノート
印刷プレビュー

反応式

HRID 856148 の反応式
[Cl:1][C:2]1[NH:3][CH:4]=[C:5]([N+:7]([O-:9])=[O:8])[N:6]=1.[C:10]1([CH3:25])[CH:15]=[CH:14][C:13]([S:16]([O:19][CH2:20][C:21]2([CH3:24])[CH2:23][O:22]2)(=[O:18])=[O:17])=[CH:12][CH:11]=1.C(#N)C>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C(OCC)(=O)C>[Cl:1][C:2]1[N:3]([CH2:24][C:21]([OH:22])([CH3:23])[CH2:20][O:19][S:16]([C:13]2[CH:14]=[CH:15][C:10]([CH3:25])=[CH:11][CH:12]=2)(=[O:18])=[O:17])[CH:4]=[C:5]([N+:7]([O-:9])=[O:8])[N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6342AcetonitrileHCID 142371942-Methyloxiran-2-ylmethyl paratoluenesulfonateHCID 178526855HCID 178526855、化合物

生成物 1

HCID 230812352-Chloro-1-[2-hydroxy-2-methyl-3-(4-methylbenzenesulfonyloxy)propyl]-4-nitroimidazole収率 70.4%

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

2-Chloro-4-nitro-1H-imidazole (1 g, 6.78 mmol), 2-methyloxiran-2-ylmethyl paratoluenesulfonate (2.46 g, 10.15 mmol), benzyl(triethyl) ammonium chloride (1.50 mg, 0.66 mmol) and acetonitrile (10 ml) were stirred under reflux for 8 hours. The reaction mixture was allowed to return to room temperature, diluted with ethyl acetate. The organic phase was washed with a saturated aqueous sodium bicarbonate solution twice, dried over magnesium sulfate and then filtered. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (methylene chloride/ethyl acetate=6/1) to afford 2-chloro-1-[2-hydroxy-2-methyl-3-(4-methylbenzenesulfonyloxy)propyl]-4-nitroimidazole (1.86 g, yield 70%) as a light yellow oil.

後処理

  1. temperatureunder reflux for 8 hours
  2. customto return to room temperature
  3. washThe organic phase was washed with a saturated aqueous sodium bicarbonate solution twice
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (methylene chloride/ethyl acetate=6/1)

出典と根拠

ORDレコード
ord-85e5f5d25b5d41e995d867a0fdf0182f
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262212B2

反応ノート

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