Methyl iodide → HCID 15580449, 화합물

HRID 615173노트

반응식

HRID 615173 반응식
[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

참가 물질

4

반응물 2

HCID 6328Methyl iodideHCID 15580438HCID 15580438, 화합물

생성물 1

HCID 15580449HCID 15580449, 화합물수율 9.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fc730d49d54c4fabbd97fb2ce9ff0f9b
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04497817

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