Methyl iodide → 5-Bromo-2-(methylthio)benzo[d]thiazole

HRID 1944687노트

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HRID 1944687 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([SH:10])=[N:7][C:6]=2[CH:11]=1.[CH2:12](N(CC)CC)C.CI>CCO>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][C:8]([S:10][CH3:12])=[N:7][C:6]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 8471TriethylamineHCID 178527757HCID 178527757, 화합물

생성물 1

HCID 28012715-Bromo-2-(methylthio)benzo[d]thiazole수율 80%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 5-bromobenzo[d]thiazole-2-thiol (24 mg, 0.098 mmol) in EtOH (1.5 mL) was added triethylamine (10 mg, 0.098 mmol) and methyliodide (14 mg, 0.098 mmol). The mixture was heated at reflux for 1.5 h. Then the mixture was extracted with dichloromethane (3×10 mL). The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated to give 5-bromo-2-(methylthio)benzothiazole 20 mg (80%).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 1.5 h
  3. extractionThen the mixture was extracted with dichloromethane (3×10 mL)
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-45a1b769159946da840d57a52d26c256
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394842B2

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