Methyl iodide → HCID 15580449、化合物

HRID 615173ノート

反応式

HRID 615173 の反応式
[NH2:1][C:2]1[CH:19]=[CH:18][C:5]2[N:6]3[CH:11]=[C:10]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)[N:9]=[C:7]3[S:8][C:4]=2[CH:3]=1.[CH3:20]I>C(O)C>[CH3:20][NH:1][C:2]1[CH:19]=[CH:18][C:5]2[N:6]3[CH:11]=[C:10]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)[N:9]=[C:7]3[S:8][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 15580438HCID 15580438、化合物

生成物 1

HCID 15580449HCID 15580449、化合物収率 9.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 50 ml of ethanol were added 500 mg of 7-amino-2-phenylimidazo[2,1-b]benzothiazole, 265 mg of methyl iodide and 260 mg of potassium carbonate anhydride and while stirring vigorously, the mixture was refluxed for 2 days. The reaction mixture was cooled and then concentrated under reduced pressure. The residue was extracted with 50 ml of ethyl acetate and the extract was washed with water, dried with anhydrous magnesium sulfate, and then the extract was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (eluant: toluene:ethyl acetate=4:1) and the obtained crystals were recrystallized from toluene to provide 50 mg of 7-methylamino-2-phenylimidazo-[2,1-b]benzothiazole.

後処理

  1. temperaturethe mixture was refluxed for 2 days
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated under reduced pressure
  4. extractionThe residue was extracted with 50 ml of ethyl acetate
  5. washthe extract was washed with water
  6. dry with materialdried with anhydrous magnesium sulfate
  7. concentrationthe extract was concentrated under reduced pressure
  8. customthe obtained crystals were recrystallized from toluene

出典と根拠

ORDレコード
ord-fc730d49d54c4fabbd97fb2ce9ff0f9b
出典データセット
uspto-grants-1985_02
特許番号
US04497817

反応ノート

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